CN110508330A - A kind of two sections of low change catalyst heating reduction processes - Google Patents
A kind of two sections of low change catalyst heating reduction processes Download PDFInfo
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- CN110508330A CN110508330A CN201910792023.3A CN201910792023A CN110508330A CN 110508330 A CN110508330 A CN 110508330A CN 201910792023 A CN201910792023 A CN 201910792023A CN 110508330 A CN110508330 A CN 110508330A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
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Abstract
The present invention relates to a kind of two sections of low change media reductive techniques, specifically a kind of two sections of low change catalyst heating reduction processes, comprising the following steps: 1) temperature rise period；2) match the hydrogen reduction stage；3) it restores initial stage: with hydrogen concentration control 0.2~0.8%, analyzing primary inlet and outlet hydrogen content after matching hydrogen；4) restore the main phase: if bed inlet temperature is stable at 160 DEG C, and bed hot(test)-spot temperature is gradually incremented by less than 220 DEG C with hydrogen concentration to 2.0%, is once mentioned hydrogen again with 0.5h stable after hydrogen；5) it restores latter stage: inlet temperature gradually being improved to 220 DEG C with the speed of 2~5 DEG C/h, and bed hot(test)-spot temperature is not higher than 230 DEG C；6) probation is restored.Operation of the present invention is simple, it is easy to accomplish, enable to two sections of low change catalyst safely, guarantee the quality, guarantor measures and completes heating reduction task, reduction efficiency is high, energy saving, has highly application value.
Description
Technical field
The present invention relates to a kind of two sections of low change media reductive techniques, specifically a kind of two sections of low change catalyst heating reduction techniques
Method.
Background technique
It is low become catalyst reduction work, to whole device can steady production play the role of vital, media reductive
Quality directly influence the stable operation of subsequent workshop section, if bad with hydrogen amount and temperature control, gently if cause catalyst to be sintered,
It is heavy then device explosion can be caused, cause work safety accident.
Therefore, for this status, there is an urgent need to develop a kind of easy to operate, it is easy to accomplish, enable to two sections of low changes
Catalyst safely, guarantee the quality, guarantor measures and completes heating reduction task, reduction efficiency is high, and two sections of energy saving low changes catalyst heatings are gone back
Original process method, to overcome the shortcomings of in currently practical application.
Summary of the invention
The embodiment of the present invention is designed to provide a kind of two sections of low change catalyst heating reduction processes, above-mentioned to solve
The problem of being proposed in background technique.
To achieve the above object, the embodiment of the present invention provides the following technical solutions:
A kind of two sections of low change catalyst heating reduction processes, comprising the following steps:
1) temperature rise period:
Using electric furnace or heat exchanger as heating source, using nitrogen as heat carrier, it is warming up to the speed of 20~30 DEG C/h from room temperature
120℃；160 DEG C are warming up to from 120 DEG C with the speed of 15 DEG C/h；Constant temperature 6h when temperature is raised to 160 DEG C, when bed bottom temp reaches
To 130 DEG C, and be higher than 30 DEG C of dew-point temperature when, heating terminates；
2) match the hydrogen reduction stage:
It restores gas concentration and requires to be H2>=55%, CO+CO2≤ 19%, O2≤ 0.2%, S≤0.1PPm, Cl-≤
0.03PPm, carrier gas air speed are 100~200h-1, system pressure 0.2MPa or less；
3) initial stage is restored:
With hydrogen concentration control 0.2~0.8%, primary inlet and outlet hydrogen content is analyzed after matching hydrogen；
4) the main phase is restored:
If bed inlet temperature is stablized at 160 DEG C, and bed hot(test)-spot temperature is gradually incremented by with hydrogen concentration extremely less than 220 DEG C
2.0%, once hydrogen is mentioned again with 0.5h stable after hydrogen；
5) latter stage is restored:
Inlet temperature is gradually improved to 220 DEG C with the speed of 2~5 DEG C/h, and bed hot(test)-spot temperature is not higher than 230 DEG C；
6) probation is restored:
It is gradually improved with hydrogen concentration with the speed of 1.0%/h to 20~30%, and bed inlet temperature is gradually increased and reaches
220 DEG C, constant temperature 1h is unchanged, and reduction terminates.
As a further solution of the present invention: in step 1), being warming up to 120 DEG C from room temperature with the speed of 25 DEG C/h.
As a further solution of the present invention: in step 2), oxygen concentration is less than 0.2% in low change furnace inlet gas, bed
First temperature of layer is 160 DEG C, and axial temperature difference is less than 30 DEG C.
As a further solution of the present invention: in step 3), the primary inlet and outlet hydrogen content of analysis per hour, and observe bed
Layer temperature rise and hydrogen consume situation.
As a further solution of the present invention: in step 4), increasing by 0.2% every time with hydrogen concentration, be often with a hydrogen
Whether the primary inlet and outlet hydrogen content of verifying is up to standard.
As a further solution of the present invention: in step 4), being equipped in the middle part of low change furnace import and two sections of low change furnaces
Press warm steam pipe line.
As a further solution of the present invention: in step 5), inlet temperature gradually being improved with the speed of 3.5 DEG C/h and is arrived
220℃。
As a further solution of the present invention: in step 6), reduction is finished, and bed temperature is reduced to 185~190 DEG C
Afterwards, and in gas sulphur, chlorine and oxygen concentration respectively reach S≤0.1PPm, Cl-≤0.03PPm、O2Start when≤0.2% requirement
Import low changing air.
Compared with prior art, the beneficial effect of the embodiment of the present invention is:
This two sections low change catalyst heating reduction processes, it is easy to operate, it is easy to accomplish, enable to two sections of low change catalyst
Safely, it guarantees the quality, guarantor's amount completion heating reduction task, reduction efficiency is high, and it is energy saving, it has highly application value.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
In order to guarantee two sections of low change catalyst safely, guarantee the quality, guarantor measure complete heating reduction task, now by this catalyst heating also
Former work division and specific heating reduction item arrange as follows:
1) personnel placement and the division of labor；
2) heating reduction medium: a) heating reduction medium is carried out with space division nitrogen；B) reduction is with methanation furnace inlet gas
Also Primordial Qi；C) start up boilers steam is used as the warm steam of pressure；
3) heating reduction process: by space division nitrogen and pressing warm steam mixing to be transported to methanation furnace through regeneration gas heat exchanger,
Or directly by space division nitrogen and press warm steam blending transportation to methanation furnace, also Primordial Qi is passed through in the import of methanation furnace；
4) catalyst heating reduction: low change catalyzer property is very active, the abnormal accidents such as overtemperature easily occurs, and this two sections
Low change catalyst heating reduction is using space division nitrogen into carrier gas, and pressurized nitrogen is touched for two sections of low changes simultaneously for 1# nitrogen compressor and 2# oxygen compressor
Matchmaker's heating reduction is used, and total tolerance is 7000m3/ h or so.
Embodiment 2
In the present embodiment, the preparation and points for attention before the heating reduction of catalyst are as follows:
A) each valve opening situation should be checked before heating reduction, whether safety is in place (to entering nitrogen tube for each correlation blind plate
The relevant process gas of line, waterpipe whole blank off separate), system is blown down, whether displacement is qualified, and whether assay work is quasi-
Standby ready, each electric thermo-couple temperature of effect indicates whether accurately, to check that each post is not used whether nitrogen valve closes again；
B) the big valve of two sections of low changing air feedwater preheater imports, the big valve in outlet, two sections of the standard-sized sheet big valves of low change import are shut
Preceding showering guilding valve requires to open two sections of low changes outlet blow valves according to heating reduction, production technology gas is forbidden to enter two sections of low changes systems
System, in order to avoid gas is mutually gone here and there, leads to serious overtemperature accident；
C) confirmation water treatment facilities work well, and are met the requirements with reaching impurity in also Primordial Qi；
D) this reduction heat source is provided using regeneration air preheater, and reduction is using the low changing air conduct after decarburization before methanation
Also Primordial Qi；
E) nitrogen pressure must control stabilization, should have pressure gauge in nitrogen system and tower entrance, and facilitate operator
Member's monitoring should take counter-measure once discovery pressure has fluctuation immediately；
F) special messenger should is responsible for being uniformly coordinated and manage during entire heating reduction, per tour should have special messenger to be responsible for operation
And analysis, and startup procedure is recorded in detail, in order to be summarized the experience and consulted；
G) thermocouple, temperature indicator, pressure gauge etc. are checked, guarantee to operate normally and is indicated.
It is as follows in the preparation and points for attention of temperature rise period in the present embodiment:
A) should check each valve opening situation before driving, each correlation blind plate whether safety in place, system blows down, displacement whether
Qualification, whether assay work is ready, and each electric thermo-couple temperature of effect indicates whether accurately again, and guarantee air speed 100~
200h-1；
B) using electric furnace or heat exchanger as heating source, using nitrogen as heat carrier, nitrogen requires oxygen concentration less than 0.2%, often
Temperature is to 120 DEG C, with the heating of 20~30 DEG C/h (preferably 25 DEG C/h) speed；When being warming up to 60 DEG C, has a small amount of absorption water and releases,
Temperature rise slows down, but the catalyst is generally not in long-time constant temperature, and ontology mechanical water is seldom (without deliberately constant temperature)；120℃
When can discharge water again, there is temperature rise to slow down phenomenon, can do at this time trial hydrogen with effect with hydrogen valve aperture and concentration relationship；
C) at 120~160 DEG C, with 15 DEG C/h heating, constant temperature 6h when temperature is raised to 160 DEG C reduces bed axial temperature difference, bed
Layer bottom temp reaches 130 DEG C, and heating terminates when higher than 30 DEG C of dew-point temperature.
It is as follows in the preparation and points for attention for matching the hydrogen reduction stage in the present embodiment:
A) condition: oxygen concentration is less than 0.2% in low change furnace inlet gas, and first temperature of bed is 160 DEG C, axial temperature difference
Less than 30 DEG C；
B) reduction gas concentration requirement: H2>=55%, CO+CO2≤ 19%, O2≤ 0.2%, S≤0.1PPm, Cl-≤
0.03PPm, the impurity such as oil-containing, carrier gas air speed are not 100~200h-1, system pressure 0.2MPa or less；Methanation inlet pressure is used
Imported valve control is stablized, and forbids to fluctuate.
It is as follows in the preparation and points for attention at reduction initial stage in the present embodiment:
Reduction initial stage can be controlled in 0.2~0.8% with hydrogen concentration, with primary inlet and outlet hydrogen content is analyzed after hydrogen, generally
In the case of the primary inlet and outlet hydrogen content of analysis per hour, to monitor hydrogen consumption in time, and observe bed temperature rise and hydrogen consumes situation；By
There is temperature change soon without apparent induction period when nitrogen makees carrier gas in the catalyst after being incorporated hydrogen, adjust
Shi Buneng acts with undue haste, and should be subject to the guidance of site technology attendant.
It is as follows in the preparation and points for attention for restoring the main phase in the present embodiment:
A) follow principle: temperature raising does not mention hydrogen, proposes hydrogen not temperature raising, less plus hydrogen, spares no effort to hydrogen, diligent analysis, as far as possible suitable air speed,
Low temperature, low hydrogen, low pressing operation；
If b) bed inlet temperature is stablized at 160 DEG C, bed hot(test)-spot temperature can gradually be incremented by less than 220 DEG C with hydrogen concentration,
It is advisable every time with increasing by 0.2%, often analyzes primary inlet and outlet hydrogen content with a hydrogen, whether increased with verifying with hydrogen amount；Match
Hydrogen can be mentioned again by stablizing the side 0.5h after hydrogen；
C) after import hydrogen content reaches 2.0%, hydrogen concentration cannot be improved again, and stabilization operates at this concentration；
D) hydrogen source should be cut off, immediately to guarantee that every bit temperature is no more than 230 if any temperature temperature runaway situation in reduction
℃；To avoid causing bed temperature runaway because of burst accident, this is equipped with pressure temperature in the middle part of low change furnace import and two sections of low change furnaces
Steam pipe line, in case of need.
It is as follows in the preparation and points for attention in reduction latter stage in the present embodiment:
The phase, there are also certain hydrogen consumptions, should grasp reduction process according to various data, phenomenon, cannot act with undue haste, cause
Erroneous judgement and overtemperature；Bed each point temperature gradually reaches unanimity at this time, and only bottom temp is high, can be gradually with 2~5 DEG C/h
(preferably 3.5 DEG C/h) speed improves inlet temperature to 220 DEG C, and bed hot(test)-spot temperature is not higher than 230 DEG C.
It is as follows in the preparation and points for attention of reduction probation in the present embodiment:
If bed is without obvious temperature rise, analysis inlet and outlet hydrogen concentration it makes no odds, be gradually increased with hydrogen concentration (with 1.0%/
H is advisable) and inlet temperature, reaching 220 DEG C until hydrogen content is increased to 20~30%, bed inlet temperature, constant temperature 1h is unchanged,
Reduction comes to an end；As during discovery have bed temperature rise suddenly with overtemperature sign, should cut off hydrogen source immediately, increase tolerance and carry out
It blows down.
It is as follows in the preparation and points for attention of light load production in the present embodiment:
A) reduction finishes, and bed temperature is reduced to after 185~190 DEG C and starts to import low changing air, gas should be analyzed before air guide
Sulphur, chlorinity in body, reach S≤0.1PPm, Cl-≤0.03PPm、O2≤ 0.2% requirement can air guide, tolerance when air guide
It should control, while pay attention to inlet temperature in indication range；
B) there is a stronger suction-operated to CO due to catalyst, when air guide can generate temperature and rise phenomenon suddenly, should increase at this time
Air guide amount quickly takes away heat, and temperature is restored normal after 0.5h；
C) the light load phase is generally 2~3 days, and load is improved after catalyst performance stabilised to be advisable.
In the present embodiment, other points for attention are as follows:
A) during entire heating reduction, bed any point temperature all no more than 230 DEG C, should generally be controlled at 220 DEG C
Left and right；As 200h is not achieved in carrier gas air speed-1, the heating reduction time can be extended；
B) gas used such as heating reduction all recycles, and wants when reverting to the middle and later periods, exit analysis has hydrogen
Pay attention to hydrogen additional amount, in order to avoid causing hydrogen concentration excessively high, needs to take measures when necessary；
C) liquid water cannot be brought into furnace in whole process, otherwise will affect intensity；
D) methanation inlet pressure is controlled with methanation outlet valve, forbids to fluctuate；
E) unusual conditions are waited in case of nitrogen interrupts or methanation system pressure oscillation is larger, it is necessary to close match hydrogen valve immediately；
After processing is normal, required to match hydrogen again according to field technician；
F) during heating reduction, each post forbids to allow without raw skill quality inspection portion using nitrogen；
G) Oxygen in Nitrogen Gas content is kept a close eye in space division post, is forbidden exceeded.
By taking SCST-231 low change catalyzer as an example, heating reduction program is as shown in table 1 below:
Table 1
This two sections low change catalyst heating reduction processes, it is easy to operate, it is easy to accomplish, enable to two sections of low change catalyst
Safely, it guarantees the quality, guarantor's amount completion heating reduction task, reduction efficiency is high, and it is energy saving, it has highly application value.
The above are merely the preferred embodiment of the present invention, it is noted that for those skilled in the art, not
Under the premise of being detached from present inventive concept, several modifications and improvements can also be made, these also should be considered as protection model of the invention
It encloses, these all will not influence the effect and patent practicability that the present invention is implemented.
Claims (8)
1. a kind of two sections of low change catalyst heating reduction processes, which comprises the following steps:
1) temperature rise period:
Using electric furnace or heat exchanger as heating source, using nitrogen as heat carrier, 120 are warming up to from room temperature with the speed of 20~30 DEG C/h
℃；160 DEG C are warming up to from 120 DEG C with the speed of 15 DEG C/h；Constant temperature 6h when temperature is raised to 160 DEG C, when bed bottom temp reaches
130 DEG C, and be higher than 30 DEG C of dew-point temperature when, heating terminates；
2) match the hydrogen reduction stage:
It restores gas concentration and requires to be H2>=55%, CO+CO2≤ 19%, O2≤ 0.2%, S≤0.1PPm, Cl-≤ 0.03PPm, carrier gas are empty
Speed is 100~200h-1, system pressure 0.2MPa or less；
3) initial stage is restored:
With hydrogen concentration control 0.2~0.8%, primary inlet and outlet hydrogen content is analyzed after matching hydrogen；
4) the main phase is restored:
If bed inlet temperature is stablized at 160 DEG C, and bed hot(test)-spot temperature is gradually incremented by less than 220 DEG C with hydrogen concentration to 2.0%,
Once hydrogen is mentioned again with 0.5h stable after hydrogen；
5) latter stage is restored:
Inlet temperature is gradually improved to 220 DEG C with the speed of 2~5 DEG C/h, and bed hot(test)-spot temperature is not higher than 230 DEG C；
6) probation is restored:
It is gradually improved with hydrogen concentration with the speed of 1.0%/h to 20~30%, and bed inlet temperature is gradually increased and reaches 220 DEG C,
Constant temperature 1h is unchanged, and reduction terminates.
2. two sections of low change catalyst heating reduction processes according to claim 1, which is characterized in that in step 1),
120 DEG C are warming up to from room temperature with the speed of 25 DEG C/h.
3. two sections of low change catalyst heating reduction processes according to claim 2, which is characterized in that in step 2,
Oxygen concentration is less than 0.2% in low change furnace inlet gas, and first temperature of bed is 160 DEG C, and axial temperature difference is less than 30 DEG C.
4. two sections of low change catalyst heating reduction processes according to claim 3, which is characterized in that in step 3),
The primary inlet and outlet hydrogen content of analysis per hour, and observe bed temperature rise and hydrogen consumption situation.
5. two sections of low change catalyst heating reduction processes according to claim 1, which is characterized in that in step 4),
Increase by 0.2% every time with hydrogen concentration, whether often verify primary inlet and outlet hydrogen content with a hydrogen up to standard.
6. two sections of low change catalyst heating reduction processes according to claim 1 or 5, which is characterized in that in step 4)
In, the warm steam pipe line of pressure is equipped in the middle part of low change furnace import and two sections of low change furnaces.
7. two sections of low change catalyst heating reduction processes according to claim 1, which is characterized in that in step 5),
Inlet temperature is gradually improved to 220 DEG C with the speed of 3.5 DEG C/h.
8. two sections of low change catalyst heating reduction processes according to claim 1 or claim 7, which is characterized in that in step 6)
In, reduction finishes, after bed temperature is reduced to 185~190 DEG C, and in gas sulphur, chlorine and oxygen concentration respectively reach S≤
0.1PPm、Cl-≤0.03PPm、O2Start to import low changing air when≤0.2% requirement.
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Application publication date: 20191129 |