CN1817459A - Simulated thermal-insulating reaction experimental method in laboratory - Google Patents
Simulated thermal-insulating reaction experimental method in laboratory Download PDFInfo
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Abstract
An experimental method and apparatus for simulating the adiabatic reaction in laboratory is characterized by that the miniature single-tube reactor is used and solid bed layer of catalytic reactor is heated according predictated value to generate an artificial temp gradient. It is suitable for the strong heat releasing reaction (alkylation, oligorization, or hydrogenation).
Description
Technical field
The present invention relates to a kind of laboratory simulation adiabatic reaction experimental technique, the particularly experimental technique of simulation chemical synthesis adiabatic reaction, and corresponding experimental provision.
" the laboratory simulation adiabatic reaction experimental technique " of the present invention's design makes the researcher utilize small-sized, miniature single tube reactor in the laboratory, obtains the basic data of the industrial reaction device design of adiabatic reaction.The present invention is according to the bed temperature rise of the solid catalysis reactions device of estimating in advance or the size of temperature drop, and the people carries out for causing thermograde, make to be reflected under this simulation adiabatic condition in reactor.Then result of the test and the laboratory purpose value that obtains compared,, revise the thermograde setting value, carry out repeatedly so repeatedly, coincide up to both according to the size of deviation.
Background technology
The exothermic heat of reaction principle: in the adiabatic heterogeneous reaction that fixed-bed tube reactor carries out, if reaction has fuel factor, reactant is from import (import) contact catalyst bed, and the heat (Q) that just responds produces:
Qi＝u·c·xi·ΔH
In the formula: the thermal discharge when Qi proceeds to i for reaction, Js-1;
U is a feed rate, Ls-1;
C is a reactant concentration, molL-1;
Conversion ratio when xi is i, %;
Δ H is the enthalpy change value, Jmol-1.
Do not consider the variations in temperature of catalyst and reactor member, the temperature rise of reaction logistics:
Δti＝Qi/(u·C)
In the formula: Δ ti is the temperature rise of reacting when proceeding to i, K;
C is the mean heat capacity of reaction logistics, Jmol-1K-1.
From import to the outlet overall temperature rise:
Δt∑＝Q/(u·C)
Q is the overall reaction heat of conversion ratio when reaching the reactor outlet conversion ratio in the formula.
Because the temperature rise that reaction heat causes, exothermic reaction is risen gradually along the reactor length temperature, i.e. there is axial temperature difference (axes) from Reactor inlet in logistics to outlet (exit): Δ taxe=|timp-texit|＞1.The size of Δ taxe depends on reaction depth.
In addition, because reactor wall inboard (inside) temperature t in is different with the wall outside (exterior) temperature t ex, and exist the temperature difference and heat to transmit, therefore cause from the outside thermograde in bed center (center), promptly exist by wall heat and transmit radially (radial) temperature difference that causes: Δ trad=|tcen-tins|＞1.Reactor diameter is big more, and the influence that wall conducts heat is more little.
For exothermic reaction, commercial plant, particularly large-scale reactor as long as reactor wall insulation measure is enough, is considered the influence that radial symmetry gradient brings hardly.The laboratory is then different, and the diameter of tubular reactor is little, and the relatively hot loss is many, can't obtain reliable experimental, therefore in order to satisfy the needs of Industrial Plant Design, require to consider the test of fuel factor, generally all carry out scale-up at the bigger pilot-plant of scale.Thereby in the thermal insulation of strictness, promptly reactor wall does not exist under the radial heat transfer condition, obtains the adiabatic reaction data, comprises the adiabatic temperature rise data of reactor out temperature and reactor, is used for industry and amplifies.Yet the data that the way that this dependence major diameter reduces the radial temperature difference influence relatively obtains still have deviation in further amplifying.
In the laboratory,, be considered to impossible or insecure for industrial adiabatic reactor provides exothermic reaction data and technical data always.Because general experimental provision lacks accurate calorimetric instrument and the effective measures that reactor wall heat is transmitted are equipped and prevented in tight thermal insulation, therefore adiabatic reaction is difficult to obtain accurately in common laboratory and amplifies applied test data for industry, and is difficult to be applied in the middle of the commercial plant.
Summary of the invention
The objective of the invention is: a kind of simulated thermal-insulating reaction experimental method in laboratory is provided,, obtains with industrial production applicable as related datas such as conversion ratio, reactor out temperatures, for industrial design provides accurate foundation by the experiment of simulation adiabatic reaction lab scale.Under the thermodynamic data (reaction heat, thermal capacitance, heat content etc.) of reaction itself is known condition, investigate the catalyst performance that uses, particularly in reaction process, reaction rate (conversion ratio) when form changing along with reaction system under the different temperatures, be the apparent kinetics data, be used for catalyst screening, and provide foundation for the design of the commercial plant of regulation catalyst.The present invention is based on such known conditions and experiment purpose, propose easy relatively laboratory simulation adiabatic reaction method.
Another object of the present invention is: for simulation adiabatic reaction test provides a kind of laboratory simulation adiabatic reaction apparatus.
The object of the present invention is achieved like this:
Laboratory simulation adiabatic reaction apparatus: comprise head tank, measuring pump, reactor and product jar.Thermometer is arranged in head tank, connect measuring pump, flowmeter and ball-and-seat on the head tank outlet line.The measuring pump outlet line compiles, and through static mixer coupled reaction device charging aperture.The reactor discharging opening has pipeline to connect the product jar.The structure of reactor is: housing is cylindric, and internal diameter highly is between the 800-1200 millimeter between the 20-40 millimeter.There is charging aperture the housing upper end, and there is discharging opening the housing lower end, and there is the thermocouple socket housing lower end, and the thermocouple that can move up and down is arranged in the thermocouple socket.The thermocouple that employing moves up and down can the interior variations in temperature along the catalyst bed layer height of observing response device.The housing outer wall is enclosed with two groups of electrical heating elements at least, is preferably in the housing outer wall and is enclosed with four groups of electrical heating elements.There are temperature survey and temperature control equipment in corresponding electrical heating elements place.
For more accurate measurement flow, the flowmeter that adopts on the head tank outlet line in this device is a glass rotameter.
In order to improve the raw material cleannes, can on the head tank outlet line, be connected with filter.
Simulated thermal-insulating reaction experimental method in laboratory of the present invention is:
A, determine the experiment purpose value: promptly determine the final Synthesis conversion that experiment need reach.
B, open electrical heating elements reactor is heated up: open the pipeline insulation heating of adiabatic reaction apparatus and the insulation heating element heater and the reactor heating element heater of reaction mass, the control reactor inlet temperatures is between 70～90 ℃, outlet temperature is controlled between 100～140 ℃, reaches and keeps said temperature.
C, charging reaction: after the reactor pre-heating temperature elevation reaches predetermined thermograde, open successively the simulation adiabatic reaction apparatus in from head tank to reactor and reactor outlet to the valve between the product jar, start measuring pump and advance reaction mass, control enters the reaction mass flow of reactor.Reaction mass arrives in the product jar through measuring pump, reactor successively and forms synthetic product.
D, adjusting Temperature Distribution: slowly spur the thermocouple at reactor middle part, observe the thermograde in beds centre.Conditioned reaction device heating element heater makes reactor keep the out temperature gradient of afore mentioned rules.
E, sampling analysis: after the thermograde in catalyst in reactor bed centre is stablized, adopt the sample data of reaction mass and synthetic product, sample data comprises: feeding temperature, each section of reactor temperature, feed rate.Calculate, analyze experiment synthetic product conversion ratio.
F, comparative conversions, adjust reaction temperature: because first experimental result can not conform to final experimental result, so deviation between palpus contrast experiment's synthetic product conversion ratio and the final Synthesis conversion of experiment purpose, suitably adjust electrical heating elements, change reactor catalyst bed temperature gradient, proceed synthetic reaction.
G, comparative conversions once more, adjust, change reactor catalyst bed temperature gradient: after reactor catalyst bed temperature gradient is stable once more, gather the sample of reaction mass and synthetic product once more, deviation between calculating, analysis and contrast experiment's synthetic product conversion ratio and the final Synthesis conversion, adjust electrical heating elements once more, change reactor catalyst bed temperature gradient, carry out synthetic reaction.
H, finish the simulation adiabatic reaction: so through over-sampling, analysis, contrast, adjust, change the reaction bed temperature gradient repeatedly, progressively approach, reach experiment synthetic product conversion ratio identical with the final synthetic product conversion ratio of experiment purpose value till, finish the laboratory simulation adiabatic reaction.Experiment finally obtains adjusted reaction bed temperature gradient data value.The reaction bed temperature gradient of Xing Chenging is near industrial production reality like this, and the situation in that this temperature range is reacted just can reach industrial situation, just can well reproduce industrial data, reaches the effect that pilot scale is amplified.
In the process of the test, contrast repeatedly and adjust, up to being reflected at the conversion ratio that " artificial temperature gradient zone " reaches, consistent with final synthetic product conversion ratio.The temperature rise that the heat that is produced forms coincide with the reactor out temperature of " artificially " creation.The lab scale of chamber and pilot scale research just can simulate industrial production data so by experiment, thereby obtain good enlarge-effect.
Experiment with computing synthetic product conversion ratio of the present invention is: the amount/unit interval inlet amount of experiment synthetic product conversion ratio=unit interval target product.
The method of change of the present invention, adjustment reactor catalyst bed temperature gradient is: if experiment synthetic product conversion ratio is higher than the final synthetic product conversion ratio of experiment purpose value, illustrate that catalyst activity is than expection level height, should be according to the value of the Δ t that sets, guaranteeing under the above-mentioned Δ t prerequisite, suitably reduce the integral value of tin and tout, Δ taxe is descended, and then x descends gradually thereupon and tends to required value gradually, and running reaches stable.Otherwise, if experiment synthetic product conversion ratio is lower than the final synthetic product conversion ratio of experiment purpose value, the catalyst activity deficiency is described, need under the condition that keeps Δ t, suitably improve tin and tout integral value, x rises thereupon gradually.Be benchmark all in the entire test, operate to keep Δ taxe=Δ t.
The time of sampling analysis of the present invention, contrast, adjustment reactor catalyst bed temperature gradient is determined like this: the reaction unit start of run is that carried out once in one hour at every interval, carries out once in every 4-12 hour after reaction unit runs well.
Core of the present invention comprises two parts:
1) temperature rise of primary Calculation do not need very accurate, can by the test progressively the temperature rise to " accurately " approach, up to the acquisition reliable result;
2) adopt the adjustable electrical heating elements heating of multiple spot outside the reactor of experimental rig, offset the reactor wall heat and scatter and disappear, logistics heats up under the effect of reaction heat effect in the reactor thereby make.
With regard to synthetic reaction, what paid close attention to is key elements such as conversion ratio and selectivity, and with regard to this method, conversion ratio is even more important, so the basis of this method is determined with conversion ratio.
Generating the nonyl phenol reaction with nonene and phenol reactant is example, and concrete computational methods are described:
Phenol and nonene alkylated reaction are exothermic reaction, and generation heat is 9.92 * 104J/mol, and solving and removing heat is the key technology of this technology with control catalyst bed reaction temperature.At first must carry out heat balance to designed process conditions, the reaction outlet temperature of obtaining must be the temperature that resin catalyst can bear, determine with this whether technology is feasible, carry out simulated test then and investigate under design condition, to turn round whether to reach the conversion ratio of expection.Figure below is that alkylated reaction heat is calculated schematic diagram, and t1 and t2 are respectively Reactor inlet and outlet temperature.Heat balance carries out according to the variation of enthalpy.The reaction process that nonene and phenol reactant generate nonyl phenol is expressed as follows:
A: nonene, B: phenol, C: nonyl phenol, D: binonylphenol
Nonene and phenol reactant generate the fixed bed adiabatic reactor heat weighing apparatus computational process of nonyl phenol:
The reaction inlet state arrives the enthalpy change Δ H1 of standard state:
ΔH1＝-Nn0×68.67(t1-25)-Nph0[47.785(t1-41)+2690+31.595(41-25)]
-Nnp0×101.2(t1-25)-Ndnp0×111.75(t1-25)———(1)
In the formula: Nn0---reaction inlet nonene molal quantity
Nph0---reaction inlet phenol molal quantity
Nnp0---reaction inlet nonyl phenol molal quantity
Ndnp0---the molal quantity of reaction inlet binonylphenol.
The hot Δ H2 of the generation of reacting under the standard state:
ΔH2＝-(Nnp1-Nnp0)×23700-(Ndnp1-Ndnp0)×33000———(2)
In the formula: Nnp1---reaction outlet nonyl phenol molal quantity
Ndnp1---reaction outlet binonylphenol molal quantity.
By standard state to the reaction discharge state enthalpy change Δ H3:
ΔH3＝Nn1×68.67(t2-25)+Nph1[47.785(t2-41)+2690+31.595(41-25)]
+Nnp1×101.2(t2-25)+Ndnp1×111.75(t2-25)————(3)
In the formula: Nn1---reaction outlet nonene molal quantity
Nph1---reaction outlet phenol molal quantity
For adiabatic reaction:
ΔH＝ΔH1+ΔH2+ΔH3＝0 ——————————(4)
Set reaction conversion ratio, raw materials components mole ratio, nonyl phenol selectivity, can obtain Nn0, Nph0, Nnp0, Ndnp0, Nn1, Nph1, Nnp1, Ndnp1.Set reactor inlet temperatures t1 again, obtain reactor outlet temperature t 2 by formula (4).
The invention has the beneficial effects as follows: adopt way of the present invention, produced beyond thought effect.In the laboratory, can finish simulated test.Break small-sized in the laboratory, miniature single tube reactor adiabatic reaction and be difficult to obtain accurately for industry and amplify applied test data, and be difficult to be applied to traditional concept in the middle of the commercial plant.In insulation fix bed reaction system, simulate industrial situation preferably, experimental data that is obtained and industrial production be actual comparativity preferably, can be directly used in the middle of the industrial design, avoid and reduced the possibility of carrying out extensive pilot scale, shortened the process of scientific research and development, also increased the space-time yield of reaction system simultaneously greatly, reduce the reaction load of catalyst, increase catalyst service life.
Method and apparatus of the present invention is particularly suitable for strong exothermal reactions such as alkylation, oligomerisation, hydrogenation.
Description of drawings
Accompanying drawing 1 is a laboratory simulation adiabatic reaction apparatus schematic diagram of the present invention, also is the simulated thermal-insulating reaction experimental method in laboratory schematic flow sheet.Head tank (1,2) has been represented two kinds of head tank forms respectively, can use wherein a kind ofly, also can two kinds uses simultaneously.
Accompanying drawing 2 is structure of reactor schematic diagrames.
The specific embodiment
Embodiment: the laboratory experiment that adopts this simulation adiabatic apparatus to carry out nonene and alkylation of phenol reaction is an example, further specifies.Consult the reaction process that nonene and phenol reactant generate nonyl phenol.
At first carry out laboratory research, determine reaction rule, and set up Mathematical Modeling according to reaction rule.This step is the basis of all working, and the data of the relevant reaction rule that this step obtained are set up the basis of Mathematical Modeling after becoming.According to experimental program and laboratory Primary Study result, determined the relation between reaction temperature, material proportion and the conversion ratio, determine that catalyst is cation resin catalyzing agent Amberlyst15, the single tube consumption is 15g, performance variable is reactor import and export temperature, distribution ratio, determine the influence of performance variable, set up Mathematical Modeling on this basis reaction.
A, determine the experiment purpose value: promptly determine the final Synthesis conversion that experiment need reach.Carry out laboratory research, determine reaction rule, and set up Mathematical Modeling according to reaction rule.This step is the basis of all working, the data of the relevant reaction rule that this step obtained, and set up Mathematical Modeling
B, pilot experiment require the nonene conversion ratio to reach nonene conversion ratio Xn 〉=94%, and nonyl phenol selectivity Sn 〉=95%, pressure are normal pressure.Nonene contacts with catalyst in reactor with phenol, carries out alkylated reaction.
According to this requirement, design and made corresponding simulation adiabatic reaction apparatus.Consult accompanying drawing 1.Comprise head tank (1), measuring pump (2), reactor (6) and product jar (7).In head tank (1), thermometer is arranged, connect measuring pump (2), glass rotameter (3) and ball-and-seat (5) on head tank (1) outlet line.On head tank (1) outlet line, be connected with filter (8).The measuring pump outlet line compiles, and through static mixer (4) coupled reaction device (6) charging aperture (9).Reactor discharging opening (13) has pipeline to connect product jar (7).Consult accompanying drawing 2.The structure of reactor is: housing (10) is for cylindrical, and internal diameter is 25 millimeters, 3 millimeters of thickness, 950 millimeters of height.In adorn 25 milliliters of fixed bed reactors, reactor adopts four groups of electrical heating elements (11) to heat, control.Reactor shell (10) Outer Tube adopts the heating tape insulation.There is the thermocouple (13) that moves up and down housing (10) lower end.
C, at first total Xn 〉=94%th, task determines that therefore the total amount of heat number of reaction generation is certain, and these heats will rely on the reaction logistics to take away, and the temperature rise by logistics just removes heat for the bed catalyst.Change phenol, nonene (mol) in the calculating than R, the overall temperature rise of the reaction logistics when obtaining different R, overall temperature rise is removed by the reaction temperature utilized of catalyst, obtains minimal reaction hop count d, rounds and obtains actual hop count D.D is big more, just can adopt less R; Conversely, R is big, and D just can lack, and calculates R=3.5 stagnation temperature and be upgraded to 140 ℃ through relatively determining repeatedly, obtains D=3, three sections adiabatic reactions of this process using just, and every section temperature rise is controlled at about 45 ℃.
D, open electrical heating elements reactor (6) is heated up: open the pipeline insulation heating of adiabatic reaction apparatus and the insulation heating element heater and the reactor heating element heater (11) of reaction mass, the control reactor inlet temperatures is between 70～90 ℃, outlet temperature is controlled between 100～140 ℃, reaches and keeps said temperature.
E, charging reaction: after reactor (6) pre-heating temperature elevation reaches predetermined thermograde, open successively the simulation adiabatic reaction apparatus in from head tank (1) to reactor (6) and reactor outlet (12) to the valve between the product jar (7), start measuring pump (2) and advance reaction mass, control enters the reaction mass flow of reactor (6).Reaction mass passes through measuring pump (2) successively, reactor (6) arrives and forms synthetic product in the product jar (7).
F, adjusting Temperature Distribution: slowly spur the thermocouple (13) at reactor middle part, observe the thermograde in beds centre.Conditioned reaction device heating element heater (11) makes reactor (6) keep the out temperature gradient of afore mentioned rules.
If experiment synthetic product conversion ratio is higher than the final synthetic product conversion ratio of experiment purpose value, illustrate that catalyst activity is than expection level height, should be according to the temperature value of the Δ t=45 that sets, guaranteeing under the above-mentioned Δ t prerequisite, suitably reduce the integral value of tin=70 and tout=115, make tin drop to 65 ℃ and tout and drop to 110, Δ taxe integral value reduces, then x descends gradually thereupon and tends to required value gradually, and running reaches stable.Otherwise, if experiment synthetic product conversion ratio is lower than the final synthetic product conversion ratio of experiment purpose value, the catalyst activity deficiency is described, need under the condition that keeps Δ t, suitably improve tin and tout integral value, x rises thereupon gradually.Be benchmark all in the entire test, operate to keep Δ taxe=Δ t.
G, sampling analysis: after the thermograde in reactor (6) inner catalyst bed centre is stablized, adopt the sample data of reaction mass and synthetic product, sample data comprises: feeding temperature, each section of reactor temperature, feed rate.Calculate, analyze experiment synthetic product conversion ratio.
H, comparative conversions, adjust reaction temperature: in experimentation, all the time pay close attention to the deviation between the final Synthesis conversion of contrast experiment's synthetic product conversion ratio and experiment purpose, constantly adjust by described method in the middle of the above-mentioned F bar, adjust electrical heating elements (11), change reactor (6) reaction bed temperature gradient, proceed synthetic reaction.
I, finish the simulation adiabatic reaction: so through over-sampling, analysis, contrast, adjust, change the reaction bed temperature gradient repeatedly, progressively approach, reach experiment synthetic product conversion ratio identical with the final synthetic product conversion ratio of experiment purpose value till, finish the laboratory simulation adiabatic reaction.Experiment finally obtains adjusted thermograde data value.
Utilize the pilot-plant condition to carry out the experiment of nonene and alkylation of phenol reaction.Be in the fixed bed reactors of φ 87 * 3.5mm promptly, load the agent of 3.8kg cation resin catalyzing, finish the contrast experiment one time at reactor.It is as follows to obtain comparative analysis as a result:
Table 1 simulation adiabatic reactor reactor test and pilot experiment analysis result
| The simulation adiabatic reaction apparatus | Pilot-plant | ||||||
| Reactor inlet temperature ℃ | Reactor outlet temperature ℃ | Nonene conversion ratio % | Nonyl phenol selectivity % | Reactor inlet temperature ℃ | Reactor outlet temperature ℃ | Nonene conversion ratio % | Nonyl phenol selectivity % |
| 80 | 125 | 94.89 | 96.58 | 80 | 126 | 94.67 | 96.35 |
By table 1 as seen, about 45 ℃, simulated test turn round under design condition and has reached the conversion ratio of expection according to the adiabatic temperature rise of reaction heat control reactor, the same experiment condition of employing on pilot-plant, and amplification effect is not obvious.
Proof laboratory simulation adiabatic reaction experiment has obtained Expected Results, obtains and the applicable related data of industrial production, can provide accurate foundation for industrial design.Further proof adopts way of the present invention, can finish simulated test in the laboratory.Break small-sized in the laboratory, miniature single tube reactor adiabatic reaction and be difficult to obtain accurately for industry and amplify applied test data, and be difficult to be applied to traditional concept in the middle of the commercial plant.
Claims (8)
1, a kind of simulated thermal-insulating reaction experimental method in laboratory is applied to the laboratory and simulates the adiabatic reaction test, it is characterized in that:
A, determine the experiment purpose value: promptly determine the final Synthesis conversion that experiment need reach,
B, open electrical heating elements reactor is heated up: open the pipeline insulation heating of adiabatic reaction apparatus and the insulation heating element heater and the reactor heating element heater of reaction mass, the control reactor inlet temperatures is between 70～90 ℃, outlet temperature is controlled between 100～140 ℃, reach and keep said temperature
C, charging reaction: after the reactor pre-heating temperature elevation reaches predetermined thermograde, open successively the simulation adiabatic reaction apparatus in from head tank to reactor and reactor outlet to the valve between the product jar, start measuring pump and advance reaction mass, control enters the reaction mass flow of reactor, reaction mass arrives in the product jar through measuring pump, reactor successively and forms synthetic product
D, regulate Temperature Distribution: slowly spur the thermocouple at reactor middle part, observe the thermograde in beds centre, conditioned reaction device heating element heater makes reactor keep the out temperature gradient of afore mentioned rules,
E, sampling analysis: after the thermograde in catalyst in reactor bed centre is stablized, adopt the sample data of reaction mass and synthetic product, sample data comprises: feeding temperature, each section of reactor temperature, feed rate, calculate, analyze experiment synthetic product conversion ratio
F, comparative conversions, adjust reaction temperature: the deviation between the final Synthesis conversion of contrast experiment's synthetic product conversion ratio and experiment purpose, adjust electrical heating elements, change reactor catalyst bed temperature gradient, proceed synthetic reaction,
G, comparative conversions once more, adjust, change reactor catalyst bed temperature gradient: after reactor catalyst bed temperature gradient is stable once more, gather the sample of reaction mass and synthetic product once more, deviation between calculating, analysis and contrast experiment's synthetic product conversion ratio and the final Synthesis conversion, adjust electrical heating elements once more, change reactor catalyst bed temperature gradient, carry out synthetic reaction
H, finish the simulation adiabatic reaction: so through over-sampling, analysis, contrast, adjust, change the reaction bed temperature gradient repeatedly, progressively approach, reach experiment synthetic product conversion ratio identical with the final synthetic product conversion ratio of experiment purpose value till, finish the laboratory simulation adiabatic reaction, experiment finally obtains adjusted thermograde data value.
2, simulated thermal-insulating reaction experimental method in laboratory as claimed in claim 1 is characterized in that: described experiment with computing synthetic product conversion ratio is:
Amount/unit interval the inlet amount of experiment synthetic product conversion ratio=unit interval target product.
3, simulated thermal-insulating reaction experimental method in laboratory as claimed in claim 1, it is characterized in that: the method for described change, adjustment reactor catalyst bed temperature gradient is: if experiment synthetic product conversion ratio is higher than the final synthetic product conversion ratio of experiment purpose value, illustrate that catalyst activity is than expection level height, should be according to the value of the Δ t that sets, guaranteeing suitably to reduce t under the above-mentioned Δ t prerequisite
InAnd t
OutIntegral value, make Δ t
AxeDescend, then x descends gradually thereupon and tends to required value gradually, and running reaches stable, otherwise,, the catalyst activity deficiency is described if experiment synthetic product conversion ratio is lower than the final synthetic product conversion ratio of experiment purpose value, need under the condition that keeps Δ t, suitably improve t
InAnd t
OutIntegral value, x rises thereupon gradually, in the entire test all to keep Δ t
Axe=Δ t is a benchmark, operates.
4, simulated thermal-insulating reaction experimental method in laboratory as claimed in claim 1, it is characterized in that: the time of described sampling analysis, contrast, adjustment reactor catalyst bed temperature gradient is determined like this: the reaction unit start of run is that carried out once in one hour at every interval, carries out once in every 4-12 hour after reaction unit runs well.
5, a kind of laboratory simulation adiabatic reaction apparatus, comprise head tank, measuring pump, reactor and product jar, it is characterized in that: thermometer is arranged in head tank, connect measuring pump on the head tank outlet line, flowmeter and ball-and-seat, the measuring pump outlet line compiles, and through static mixer coupled reaction device charging aperture, the reactor discharging opening has pipeline to connect the product jar, the structure of reactor is: housing is cylindric, internal diameter highly is between the 800-1200 millimeter between the 20-40 millimeter, and there is charging aperture the housing upper end, there is discharging opening the housing lower end, there is the thermocouple socket housing lower end, has the thermocouple that can move up and down, housing outer wall to be enclosed with two groups of electrical heating elements at least in the thermocouple socket, there are temperature survey and temperature control equipment in corresponding electrical heating elements place.
6, laboratory simulation adiabatic reaction apparatus as claimed in claim 5 is characterized in that: the housing outer wall is enclosed with four groups of electrical heating elements.
7, as claim 5 or 6 described laboratory simulation adiabatic reaction apparatus, it is characterized in that: the flowmeter that adopts on the head tank outlet line is a glass rotameter.
8, as claim 5 or 6 described laboratory simulation adiabatic reaction apparatus, it is characterized in that: on the head tank outlet line, be connected with filter.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008080365A1 (en) * | 2006-12-29 | 2008-07-10 | Accelergy Shanghai R & D Center Co., Ltd. | High throughput development method for catalytic hydroprocessing of dirty feedstocks |
| CN108535315A (en) * | 2018-03-30 | 2018-09-14 | 沈阳化工研究院有限公司 | A kind of measurement method and device of non-isothermal reaction process calorimetric |
| CN112782221A (en) * | 2020-12-25 | 2021-05-11 | 沈阳化工研究院有限公司 | Calorimetric test method for photocatalytic reaction |
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| DE3336750A1 (en) * | 1982-10-15 | 1984-04-19 | Idemitsu Kosan Co., Ltd., Tokyo | REACTOR |
| SU1269824A1 (en) * | 1985-01-04 | 1986-11-15 | Предприятие П/Я Р-6711 | Apparatus for automatic controlling of temperature conditions in the reactor for testing catalysts |
| FR2807746B1 (en) * | 2000-04-13 | 2002-12-13 | Air Liquide | METHOD FOR PRODUCING A MIXTURE COMPRISING HYDROGEN AND CO |
| US20020071798A1 (en) * | 2000-07-12 | 2002-06-13 | Decourcy Michael Stanley | Laboratory Scale reaction systems |
| CN2429254Y (en) * | 2000-07-21 | 2001-05-09 | 中国科学院大连化学物理研究所 | Pulse micro-reactor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008080365A1 (en) * | 2006-12-29 | 2008-07-10 | Accelergy Shanghai R & D Center Co., Ltd. | High throughput development method for catalytic hydroprocessing of dirty feedstocks |
| CN108535315A (en) * | 2018-03-30 | 2018-09-14 | 沈阳化工研究院有限公司 | A kind of measurement method and device of non-isothermal reaction process calorimetric |
| CN108535315B (en) * | 2018-03-30 | 2023-12-15 | 沈阳化工研究院有限公司 | Method and device for measuring calorimetric heat in non-isothermal reaction process |
| CN112782221A (en) * | 2020-12-25 | 2021-05-11 | 沈阳化工研究院有限公司 | Calorimetric test method for photocatalytic reaction |
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