CN108097175A - Formaldehyde catalyst contrast experiment's self-balancing consersion unit - Google Patents

Formaldehyde catalyst contrast experiment's self-balancing consersion unit Download PDF

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Publication number
CN108097175A
CN108097175A CN201810093345.4A CN201810093345A CN108097175A CN 108097175 A CN108097175 A CN 108097175A CN 201810093345 A CN201810093345 A CN 201810093345A CN 108097175 A CN108097175 A CN 108097175A
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CN
China
Prior art keywords
conduction oil
heat conduction
balancing
heat
reactor
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Pending
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CN201810093345.4A
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Inventor
高福祥
陈隽
杨勇
曾真
陈莉
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XINJIANG MARKOR CHEM Co Ltd
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XINJIANG MARKOR CHEM Co Ltd
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Priority to CN201810093345.4A priority Critical patent/CN108097175A/en
Publication of CN108097175A publication Critical patent/CN108097175A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/001Controlling catalytic processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • B01J8/067Heating or cooling the reactor
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/27Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
    • C07C45/29Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation of hydroxy groups
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00106Controlling the temperature by indirect heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00539Pressure

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The present invention relates to COMPARATIVE CATALYST's experimental technique fields.The present invention provides a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit, including the reaction member being connected and conduction oil unit;Reaction member includes the reactor with shell side.Conduction oil unit includes heat conduction oil tank, Heat-transfer Oil Pump, electric heater for heat conduction oil, heat conduction oil cooler;Heat conduction oil tank is connected via Heat-transfer Oil Pump, electric heater for heat conduction oil with the shell side lower part of reactor, and the shell side top of reactor is connected with heat conduction oil cooler, and heat conduction oil cooler is connected with heat conduction oil tank;Reactor bottom is equipped with heat-conducting oil heating coil pipe.This COMPARATIVE CATALYST tests self-balancing consersion unit and is primarily adapted for use in the contrast test of formaldehyde catalyst, while is also applied for the contrast test of various tubular reaction catalyst.Self-balancing can be realized for highly exothermic, middle heat release, weak-exothermic reaction.

Description

Formaldehyde catalyst contrast experiment's self-balancing consersion unit
Technical field
The present invention relates to COMPARATIVE CATALYST's experimental technique fields, and in particular to a kind of formaldehyde catalyst contrast experiment self-balancing Consersion unit.
Background technology
Formaldehyde catalyst species is various at present, but the really research to the proportioning and filling scheme of catalyst and few.Row The big portion of heat transmission of tubular reactor is realized using thermosiphon principle, but is set for the reaction of COMPARATIVE CATALYST's experimental provision It is standby, it not only needs to carry out the comparison of two kinds of catalyst under the same conditions, while also to realize in different catalyst exotherm rings Heat under border removes, and can be continuously improved and reduce heat and temperature that reaction is removed according to the needs of reaction process.Catalysis Agent uses the active and service life not only to depend on the active component with catalyst, while also has with the proportioning of catalyst and filling scheme It closes.
Prepn. of formaldehyde by oxidation of methanol catalyst is tested under identical process conditions, could preferably go out good catalyst And loading method, so it is extremely necessary to invent a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit, Be primarily adapted for use in the contrast test of formaldehyde catalyst, be for prepn. of formaldehyde by oxidation of methanol successive reaction contrast experiment's modular in design, The contrast test of various tubular reaction catalyst is also applied for simultaneously.It can be real for highly exothermic, middle heat release, weak-exothermic reaction Existing Self-balancing.
For achieving the above object, the present invention provides following technical scheme:
A kind of formaldehyde catalyst contrast experiment self-balancing consersion unit, including reaction member and conduction oil unit;Reaction is single Member includes the reactor with shell side, and conduction oil unit includes heat conduction oil tank, Heat-transfer Oil Pump, electric heater for heat conduction oil, conduction oil Cooler;Heat conduction oil tank is connected via Heat-transfer Oil Pump, electric heater for heat conduction oil with the shell side lower part of reactor, the shell of reactor Journey top is connected with heat conduction oil cooler, and heat conduction oil cooler is connected with heat conduction oil tank.
Further, the reactor bottom is equipped with heat-conducting oil heating coil pipe.
Further, the heat conduction oil cooler is connected by nitrogen pipeline with source nitrogen, is set in the nitrogen pipeline There is nitrogen Staged cotrol valve group.
Further, the conduction oil unit further includes water tank, and the water tank is connected with the heat conduction oil cooler It is logical.
Further, deionized water is loaded in the water tank, the heat conduction oil cooler top is equipped with tube sheet, described The lower part liquid level of water tank is concordant with the heat conduction oil cooler upper tube sheet.
Further, the reactor is shell and tube reactor.
Further, two bundle of reaction tubes are evenly distributed in the shell side of the reactor, two bundle of reaction tubes is interior respectively Catalyst added with different model is equipped with conduction oil between the shell side and the bundle of reaction tubes.
Further, temperature, pressure instrumentation are equipped in the reactor.
Further, the reactor is connected with the process gas outlet of prepn. of formaldehyde by oxidation of methanol process units.
Further, the operating pressure scope of this consersion unit is 0~100Kpa, and operating temperature range is 260~350 ℃;Conduction oil operating temperature range is 260~300 DEG C.
From the foregoing, it will be observed that contrast experiment's self-balancing reactor of the present invention, for weak-exothermic reaction, reaction thermal discharge itself is not It is enough, it is difficult to by the realization of heat conduction oil gasification to the control of temperature ± 1 DEG C, it is necessary to which additional heat, this reactor bottom set heat conduction Oily heating coil supplements insufficient heat, ensures heat conduction oil gasification, realizes the self-balancing control of reactor heat constant temperature system, profit Repeats itself is realized with heat-conduction oil heat siphon principle;For middle exothermic reaction, heat-conducting oil heating coil pipe is closed, by reacting itself Heat release, realize conduction oil gasification equilibrium, realize the control to temperature ± 1 DEG C, without additional heat, utilize heat-conduction oil heat siphon Principle realizes repeats itself;For highly exothermic reaction, conduction oil largely gasifies, and by heat conduction oil cooler, carries out refrigerated separation, Repeats itself is realized using heat-conduction oil heat siphon principle.The process gas of reactor and prepn. of formaldehyde by oxidation of methanol process units exports phase Connection, tubulation share a shell side, are conduction oil of the same race in shell side, are carried out pair by said structure with realizing same process condition Than experiment.
Description of the drawings
Fig. 1 is the general flow chart of one embodiment of formaldehyde catalyst contrast experiment's self-balancing consersion unit of the present invention;
Fig. 2 is the heat-conducting oil heating of the reactor bottom of formaldehyde catalyst contrast experiment's self-balancing consersion unit of the present invention Coil pipe schematic diagram.
Specific embodiment
Below in conjunction with attached drawing, the forgoing and additional technical features and advantages are described in more detail.
As shown in Figure 1:A kind of formaldehyde catalyst contrast experiment self-balancing consersion unit, including reaction member and conduction oil list Member;Reaction member include with shell side reactor R1001, conduction oil unit include heat conduction oil tank V-32, Heat-transfer Oil Pump P-31, Electric heater for heat conduction oil H-33, heat conduction oil cooler HE-34;Heat conduction oil tank V-32 adds via Heat-transfer Oil Pump P-31, conduction oil electricity Hot device H-33 is connected with the shell side lower part of reactor R1001, and the shell side top of reactor is connected with heat conduction oil cooler HE-34 Logical, heat conduction oil cooler HE-34 is connected with heat conduction oil tank V-32.
Preferably, reactor bottom is equipped with heat-conducting oil heating coil pipe.
Preferably, heat conduction oil cooler HE-34 is connected by nitrogen pipeline with source nitrogen (not shown), nitrogen tube Road is equipped with nitrogen Staged cotrol valve group FV306A/FV306B.
Preferably, conduction oil unit further includes water tank V-30, and water tank V-30 is connected with heat conduction oil cooler HE-34 It is logical.
Preferably, deionized water is loaded in water tank V-30, heat conduction oil cooler HE-34 tops are equipped with tube sheet, water storage The lower part liquid level of tank is concordant with heat conduction oil cooler upper tube sheet.
Preferably, reactor is shell and tube reactor.
Preferably, two bundle of reaction tubes are evenly distributed in the shell side of reactor, difference is added with respectively in two bundle of reaction tubes The catalyst of model is equipped with conduction oil between shell side and bundle of reaction tubes.
Preferably, temperature instrument TI112, TI212, TI111, TI210, pressure instrumentation are equipped in reactor PI113、PI213、PI110、PI211。
Preferably, reactor is connected with the process gas outlet of prepn. of formaldehyde by oxidation of methanol process units.
Preferably, the operating pressure scope of this consersion unit is 0~100Kpa, and operating temperature range is 260~350 DEG C; Conduction oil operating temperature range is 260~300 DEG C.
Below in conjunction with the present invention a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit an exemplary embodiments, The consersion unit of the present invention is described in detail, wherein:
1. reaction member:
Process gas enters the end socket of reactor R1001 shell sides, and end socket is uniformly divided into equalization in end socket inner route clapboard Two parts, each section are equipped with the bundle of reaction tubes of different catalysts, with being connected with conduction oil heat exchange in reactor R1001 shell sides, After reaching reaction temperature, process gas is reacted under the effect of the catalyst, after reaction product is entered by shell-side outlet end socket System.
Temperature instrument TI112, TI212, TI111, TI210, pressure are equipped in reactor R1001 shell sides inlet and outlet end socket Tension gauge table PI113, PI213, PI110, PI211, be equipped between upper and lower shell-side head pressure differential detection instrument PDI316, PDI321 can realize the accurate metering of pressure and temp.Be equipped in bundle of reaction tubes 9 groups of temperature temperature measurement component TE101/TE201, TE102/TE202、TE103/TE203、TE104/TE204、TE105/TE205、TE106/TE206、TE107/TE207、 TE108/TE208, TE109/TE209 can detect top-down 9 groups of temperature, and pass through at distribution type control system (DCS) Reason, final displays temperature dot chart, and show hot(test)-spot temperature position.
Reactor feed gas exported product gas should be equipped with flow-meter (not in this reactor), combination temperature detector Table TI111, TI210, pressure instrumentation PI110, PI211, pressure differential detection instrument PDI316, PDI321, pass through above-mentioned instrument Data acquisition can be carried out to reaction process.
2. conduction oil unit:
Conduction oil transport system is by heat conduction oil tank V-32, Heat-transfer Oil Pump P-31, electric heater for heat conduction oil H-33, heat conduction oil cooling But the compositions such as device HE-34, conduction oil are stored in heat conduction oil tank V-32, are driven initial stage, after being pressurizeed by Heat-transfer Oil Pump P31, by Electric heater for heat conduction oil H-33 is heated, and is sent into the shell side of reactor R1001 lower parts, after heating up in shell side to catalyst, Reactor R1001 shell sides are left from shell side top and enter heat conduction oil cooler HE-34, are cooled down in heat conduction oil cooler HE-34 After return to heat conduction oil tank V-32, so cycle.
In reactor after normal reaction, Heat-transfer Oil Pump P-31 and electric heater for heat conduction oil H-33 are closed, and open HV-327, Conduction oil carries out normal circulation according to thermosiphon principle.
For weak-exothermic reaction, reaction thermal discharge itself is inadequate, it is difficult to be realized by heat conduction oil gasification to temperature ± 1 DEG C Control is, it is necessary to which additional heat, this reactor R1001 pass through such form, mend there is provided reactor bottom heat-conducting oil heating coil pipe Insufficient heat is filled, ensures heat conduction gasification, realizes the self-balancing control of reactor heat constant temperature system.It is former using heat-conduction oil heat siphon Reason realizes repeats itself.
For middle exothermic reaction, conduction oil coil pipe heater is closed, by reacting the heat release of itself, realizes heat conduction oil gasification Balance, realizes the control to temperature ± 1 DEG C, and without additional heat, repeats itself is realized using heat-conduction oil heat siphon principle.
For highly exothermic reaction, conduction oil largely gasifies, and by heat conduction oil cooler HE-34, is cooled down, utilizes heat conduction Oily thermosiphon principle realizes repeats itself.
Reactor R1001 can realize the autobalance of conduction oil gasification temperature, pass through heat conduction oil cooler HE-34 tops The nitrogen Staged cotrol valve group FV306A/FV306B of setting adjusts conduction oil top nitrogen pressure, realizes to heat conduction oil gasification pressure The balance control of power, automatically controls so as to fulfill to reactor R1001 reaction temperatures with the process of reaction.
Reactor R1001 can realize the balance Control Scheme of heat conduction oil cooler cooling medium, in water tank V-30 Deionized water is saved, the lower part liquid level of water tank V-30 is concordant with heat conduction oil cooler HE-34 upper tube sheets, when conduction oil is by gas After change, gas cools down inside heat conduction oil cooler HE-34, and cooler shell side water is gasified, and the vapor of gasification is in efferent duct Water is cooled into road, is returned in water tank V-30, is controlled so as to fulfill self-balancing.
The foregoing is merely a prefered embodiment of the invention, is merely illustrative for the purpose of the present invention, and not restrictive.This The structure of each component and connection mode etc. can be all varied from invention, every on the basis of technical solution of the present invention The equivalents of progress and improvement should not be excluded outside protection scope of the present invention.

Claims (10)

1. a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit, which is characterized in that including reaction member and conduction oil list Member;The reaction member includes the reactor with shell side;The conduction oil unit includes heat conduction oil tank, Heat-transfer Oil Pump, heat conduction Oily electric heater, heat conduction oil cooler;The heat conduction oil tank via the Heat-transfer Oil Pump, the electric heater for heat conduction oil with it is described The shell side lower part of reactor is connected, and the shell side top of the reactor is connected with the heat conduction oil cooler, the heat conduction Oil cooler is connected with the heat conduction oil tank.
2. a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit as described in claim 1, which is characterized in that described anti- Device bottom is answered to be equipped with heat-conducting oil heating coil pipe.
3. a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit as described in claim 1, which is characterized in that described to lead Hot oil cooler is connected by nitrogen pipeline with source nitrogen, and the nitrogen pipeline is equipped with nitrogen Staged cotrol valve group.
4. a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit as described in claim 1, which is characterized in that described to lead Deep fat unit further includes water tank, and the water tank is connected with the heat conduction oil cooler.
A kind of 5. formaldehyde catalyst contrast experiment self-balancing consersion unit as claimed in claim 4, which is characterized in that the storage Be loaded with deionized water in water pot, the heat conduction oil cooler top is equipped with tube sheet, the lower part liquid level of the water tank with it is described Heat conduction oil cooler upper tube sheet is concordant.
6. a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit as described in claim 1, which is characterized in that described anti- It is shell and tube reactor to answer device.
7. a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit as claimed in claim 6, which is characterized in that described anti- It answers and two bundle of reaction tubes is evenly distributed in the shell side of device, be added with the catalyst of different model in two bundle of reaction tubes respectively, Conduction oil is equipped between the shell side and the bundle of reaction tubes.
8. a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit as claimed in claim 6, which is characterized in that described anti- It answers and temperature instrument, pressure instrumentation is equipped in device.
9. a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit as described in claim 1, which is characterized in that described anti- Device is answered to be connected with the process gas outlet of prepn. of formaldehyde by oxidation of methanol process units.
10. a kind of formaldehyde catalyst contrast experiment self-balancing consersion unit as described in claim 1 to 9 is any, feature exist In the operating pressure scope of this consersion unit is 0~100Kpa, and operating temperature range is 260~350 DEG C;Conduction oil operation temperature It is 260~300 DEG C to spend scope.
CN201810093345.4A 2018-01-31 2018-01-31 Formaldehyde catalyst contrast experiment's self-balancing consersion unit Pending CN108097175A (en)

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