CN103977843B - A kind of method of methyl alcohol catalyst heating reduction - Google Patents
A kind of method of methyl alcohol catalyst heating reduction Download PDFInfo
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- CN103977843B CN103977843B CN201410226974.1A CN201410226974A CN103977843B CN 103977843 B CN103977843 B CN 103977843B CN 201410226974 A CN201410226974 A CN 201410226974A CN 103977843 B CN103977843 B CN 103977843B
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Abstract
The present invention relates to revivification of catalyst technology, be specially a kind of method of methyl alcohol catalyst heating reduction.Solve the technical problem that current methyl alcohol catalyst easily " is burnt " in reduction process.A method of operating for methyl alcohol catalyst heating reduction, comprises the following steps: (a) temperature rise period; (b) reduction phase initial stage; C () is reduced the main phase; D () is reduced latter stage; (e) constant temperature stage.This method is the heating reduction that can be used for methyl alcohol catalyst in chemical enterprise methyl alcohol, alcohol hydrocarbylation process, can effectively control heating rate and water yield, avoids " burning " catalyst, ensures the activity after media reductive.
Description
Technical field
The present invention relates to revivification of catalyst technology, be specially a kind of method of methyl alcohol catalyst heating reduction.
Background technology
Present fertilizer enterprises generally uses Cu-Zn-Al series catalysts when carrying out methanol-fueled CLC, in oxidation state before this series catalysts does not reduce, is by high-purity C u (NO
3)
2, Zn (NO
3)
2be dissolved in Na
2cO
3obtain (Cu, Zn) by coprecipitation in solution
2(OH)
2cO
3precipitation, then adds Al
2o
3and Cr
2o
3deng the cylinder granule of the loose structure that element is formed through high temperature, and methanol-fueled CLC needs elemental copper as reaction media, therefore needs to be reduced rear use.Methyl alcohol catalyst heating reduction is exothermic reaction (other conversion, synthetic catalyst heating reduction are all the endothermic reaction), if heating rate and thermal discharge can not be controlled exactly in heating reduction process, be easy to the situation causing catalyst steep temperature rise and " burning ", this happens occasionally in many manufacturers, not that catalyst is scrapped, be exactly active not all right reduction of service life, and the heating reduction scheme key control point that catalyst producer provides and heating rate all fuzzyyer, be unfavorable for operation.
For these reasons, need to improve methyl alcohol catalyst heating reduction, make catalyst avoid " being burnt " by high temperature and scrapping, to extend its service life in reduction process.
Summary of the invention
The technical problem that the present invention easily " is burnt " in reduction process for solving current methyl alcohol catalyst, provides a kind of method of methyl alcohol catalyst heating reduction.
The present invention realizes by the following technical solutions: a kind of method of operating of methyl alcohol catalyst heating reduction, comprises the following steps: (a) temperature rise period; Reaction system rises to 70 DEG C by room temperature, and catalyst stratification temperature difference is 0 DEG C, heating rate 15-20 DEG C/h, time 3 ~ 4h; (b) reduction phase initial stage; First stage, catalyst layer hot(test)-spot temperature rises to 80 DEG C by 70 DEG C, and catalyst stratification temperature differs from 5 DEG C, programming rate rate 0-5 DEG C/h, Chu Shui Liang≤1 ~ 3Kg/ ton catalyst/h, time 2 ~ 3h; Second stage, catalyst layer hot(test)-spot temperature rises to 95 DEG C by 80 DEG C, catalyst stratification temperature difference 10-15 DEG C, programming rate rate 0-1 DEG C/h, Chu Shui Liang≤3 ~ 5Kg/ ton catalyst/h, time 20 ~ 25h; C () is reduced the main phase; First stage, catalyst layer hot(test)-spot temperature rises to 120 DEG C by 95 DEG C, catalyst stratification temperature difference 5-10 DEG C, heating rate 1-3 DEG C/h, Chu Shui Liang≤2 ~ 4Kg/ ton catalyst/h, time 15 ~ 20h; Second stage, catalyst layer hot(test)-spot temperature rises to 140 DEG C by 120 DEG C, and catalyst stratification temperature differs from 5 DEG C, heating rate 0-1 DEG C/h, Chu Shui Liang≤3 ~ 5Kg/ ton catalyst/h, time 20 ~ 25h; Phase III, catalyst layer hot(test)-spot temperature rises to 160 DEG C by 140 DEG C, catalyst stratification temperature difference 0-5 DEG C, heating rate 1 ~ 3 DEG C/h, Chu Shui Liang≤2 ~ 4Kg/ ton catalyst/h, time 10 ~ 15h; D () is reduced latter stage; First stage, catalyst layer hot(test)-spot temperature rises to 200 DEG C by 160 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 3-10 DEG C/h, Chu Shui Liang≤1 ~ 3Kg/ ton catalyst/h, time 5 ~ 10h; Second stage, catalyst layer hot(test)-spot temperature rises to 240 DEG C by 200 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 10 DEG C/h, Chu Shui Liang≤1 ~ 2Kg/ ton catalyst/h, time 4h; (e) constant temperature stage; Temperature range is 240 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 0 DEG C/h, Chu Shui Liang≤2Kg/h, and the time keeps 2h.Above in each step, all require that keeping system pressure is 5.0Mpa, systemic circulation tolerance keeps 2000h
-1volume space velocity, H in system gas
2content with volume fraction calculating for 70%.
Heating reduction process uses qualified virgin gas (namely synthesizing tonifying Qi), H in gas
2content about 70% (volume fraction), all the other compositions are N
2, CO and CO
2content does not almost have, and avoiding catalyst so dramatically has active rear methyl alcohol heat of reaction generation to cause catalyst sudden temperature rise (if gas uses decarburization after-purification gas, containing CO% and CO of 1.0% ~ 2.0% in gas in partial reduction
2%, has CO+2H
2=CH
3oH+QCO
2+ 3H
2=CH
3oH+H
2o+Q two strong exothermal reactions occur).
Sort according to metal active: K, Ca, Na, Mg, Al, Zn, Fe, Se, Pb come before H.The specific activity H of Zn and Al is strong, and the specific activity H of Cu is weak, and therefore the reduction reaction of CuO only occurs general reduction reaction:
CuO+H
2=Cu+H
2O+86.5KJ/mol
In reduction process, generate that the water yield is about catalyst weight about 20%, various model catalyst is with Cu content difference to some extent, wherein chemical water accounts for 8% ~ 10%, mechanical water accounts for 10% ~ 13%, therefore the key of copper-based catalysts reduction controls reduction reaction speed i.e. programming rate, the amount of water is generated conversely i.e. water yield controls heating rate and system reducing reaction producing heat, especially in two the water outlet peak periods going out mechanical water and chemical water by reduction reaction.Arrhenius equation: k=Ae
-Ea/RTit is described that chemical reaction rate (k) and the relation between temperature (T) and reaction activity Ea.Certain for its activation energy of certain chemical reaction, so when reaction temperature heat energy RT reaches or surmounts reaction activity Ea needed for material, chemical reaction rate leaps, be swift in response and carry out, that is a large amount of water will be generated, release a large amount of heats simultaneously, at this moment need strictly to control reaction rate, otherwise heat too much will cause catalyst temperature rise to accelerate, temperature rise stimulates again quickening reaction rate, produce more heat, form chain reaction, cause catalyst temperature to rise and " burning " very soon.According to a large amount of practical observations, the reduction process of catalyst of the present invention has 80 DEG C ~ 95 DEG C and 120 DEG C ~ 140 DEG C to be two water outlet peak period temperature ranges, therefore near these two temperature ranges, adopt temperature range of the present invention and heating rate effectively can control the speed of reduction reaction, make catalyst can not because of reaction in liberated heat and " being burnt "; The heating rate simultaneously adopted in other step and temperature range are also for whole reduction reaction is served, and ensure carrying out smoothly of whole reduction reaction; Catalyst layering relies on cold shock gas by force catalyst layer to be divided into two parts by temperature difference, avoid whole catalyst to reach reaction peak temperature and water yield is excessive simultaneously, reaction heat gathers and catalyst sudden temperature rise, and reaction heat can not be taken out of and " burning " catalyst by circulating flow rate in time.Catalyst is divided into two parts pulls open 10 ~ 15 DEG C of temperature difference intentionally, reduces water yield per hour, makes reduction reaction more easy to control.Reduce along with 160 DEG C of water outlets later and progressively turn down and close cold shock, eliminating axial temperature difference.
In the present invention, whole heating reduction process has regulations to abide by, and speed is moderate, can complete the work of catalyst heating reduction smoothly.
Further, when keeping system pressure and systemic circulation tolerance stable, heating rate speed in each stage should be adjusted according to water yield size, thus within the scope of each phases-time extend or shorten the heating reduction time; For reduction initial stage second stage, namely catalyst layer hot(test)-spot temperature rises to 95 DEG C by 80 DEG C, and reduce main phase second stage, namely catalyst layer hot(test)-spot temperature rises to 140 DEG C of these two stages by 120 DEG C, by keeping constant temperature and the mode combined that heats up, make water yield can not exceed this stage water yield requirement; Described systemic circulation tolerance refers to by volume flow 0.5m
3/ min/ ton catalyst.
Should according to the size of the water yield determination programming rate of each stage of reaction in actual heating reduction process, in actual reduction process, per half an hour discharges water and once weighs, for each stage in reduction, once more than 1.5 ~ 2Kg/ ton catalyst/half h, constant temperature half an hour is to observe water yield next time, generally only has the situation that just to there will be water yield and increase suddenly near two water outlet peak temperature, therefore must note, also would rather to avoid temperature heat " surplus " and reaction is carried out in a large number by constant temperature, after water yield affects too greatly media reductive, active structure is formed, impact is active, therefore each stage of heating up particularly reduces initial stage second stage and the main phase second stage of reduction, and temperature-rise period is one and heats up and the process of constant temperature dynamic bind, ensures that water yield is no more than corresponding requirements.
This process is the Novel operating method of summarizing the experience in conjunction with working practice according to reduction reaction principle, can be used for the heating reduction of methyl alcohol catalyst in chemical enterprise methyl alcohol, alcohol hydrocarbylation process, heating rate and water yield can be effectively controlled according to the program, avoid " burning " catalyst, ensureing the activity after media reductive, is a kind of simple and practical process.
Detailed description of the invention
The method of operating of embodiment 1 one kinds of methyl alcohol catalyst heating reductions, comprises the following steps: (a) temperature rise period; Reaction system rises to 70 DEG C by room temperature, and catalyst stratification temperature difference is 0 DEG C, heating rate 15-20 DEG C/h, time 3h; (b) reduction phase initial stage; First stage, catalyst layer hot(test)-spot temperature rises to 80 DEG C by 70 DEG C, and catalyst stratification temperature differs from 5 DEG C, programming rate rate 0-5 DEG C/h, Chu Shui Liang≤1Kg/ ton catalyst/h, time 3h; Second stage, catalyst layer hot(test)-spot temperature rises to 95 DEG C by 80 DEG C, and catalyst stratification temperature differs from 10 DEG C, programming rate rate 0-1 DEG C/h, Chu Shui Liang≤3Kg/ ton catalyst/h, time 25h; C () is reduced the main phase; First stage, catalyst layer hot(test)-spot temperature rises to 120 DEG C by 95 DEG C, and catalyst stratification temperature differs from 5 DEG C, heating rate 1-3 DEG C/h, Chu Shui Liang≤2Kg/ ton catalyst/h, time 20h; Second stage, catalyst layer hot(test)-spot temperature rises to 140 DEG C by 120 DEG C, and catalyst stratification temperature differs from 5 DEG C, heating rate 0-1 DEG C/h, Chu Shui Liang≤3Kg/ ton catalyst/h, time 25h; Phase III, catalyst layer hot(test)-spot temperature rises to 160 DEG C by 140 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 1 ~ 3 DEG C/h, Chu Shui Liang≤2Kg/ ton catalyst/h, time 15h; D () is reduced latter stage; First stage, catalyst layer hot(test)-spot temperature rises to 200 DEG C by 160 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 3-10 DEG C/h, Chu Shui Liang≤1Kg/ ton catalyst/h, time 10h; Second stage, catalyst layer hot(test)-spot temperature rises to 240 DEG C by 200 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 10 DEG C/h, Chu Shui Liang≤1Kg/ ton catalyst/h, time 4h; (e) constant temperature stage; Temperature range is 240 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 0 DEG C/h, Chu Shui Liang≤2Kg/h, and the time keeps 2h.Above in each step, all require that keeping system pressure is 5.0Mpa, systemic circulation tolerance keeps 2000h
-1volume space velocity, H in system gas
2content accounts for 70%(volume fraction).
The method of operating of embodiment 2 one kinds of methyl alcohol catalyst heating reductions, comprises the following steps: (a) temperature rise period; Reaction system rises to 70 DEG C by room temperature, and catalyst stratification temperature difference is 0 DEG C, heating rate 15-20 DEG C/h, time 4h; (b) reduction phase initial stage; First stage, catalyst layer hot(test)-spot temperature rises to 80 DEG C by 70 DEG C, and catalyst stratification temperature differs from 5 DEG C, programming rate rate 0-5 DEG C/h, Chu Shui Liang≤3Kg/ ton catalyst/h, time 2h; Second stage, catalyst layer hot(test)-spot temperature rises to 95 DEG C by 80 DEG C, and catalyst stratification temperature differs from 15 DEG C, programming rate rate 0-1 DEG C/h, Chu Shui Liang≤5Kg/ ton catalyst/h, time 20h; C () is reduced the main phase; First stage, catalyst layer hot(test)-spot temperature rises to 120 DEG C by 95 DEG C, catalyst stratification temperature difference 5-10 DEG C, heating rate 1-3 DEG C/h, Chu Shui Liang≤4Kg/ ton catalyst/h, time 15h; Second stage, catalyst layer hot(test)-spot temperature rises to 140 DEG C by 120 DEG C, and catalyst stratification temperature differs from 5 DEG C, heating rate 0-1 DEG C/h, Chu Shui Liang≤5Kg/ ton catalyst/h, time 20h; Phase III, catalyst layer hot(test)-spot temperature rises to 160 DEG C by 140 DEG C, and catalyst stratification temperature differs from 5 DEG C, heating rate 1 ~ 3 DEG C/h, Chu Shui Liang≤4Kg/ ton catalyst/h, time 10h; D () is reduced latter stage; First stage, catalyst layer hot(test)-spot temperature rises to 200 DEG C by 160 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 3-10 DEG C/h, Chu Shui Liang≤3Kg/ ton catalyst/h, time 5h; Second stage, catalyst layer hot(test)-spot temperature rises to 240 DEG C by 200 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 10 DEG C/h, Chu Shui Liang≤2Kg/ ton catalyst/h, time 4h; (e) constant temperature stage; Temperature range is 240 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 0 DEG C/h, Chu Shui Liang≤2Kg/h, and the time keeps 2h.Above in each step, all require that keeping system pressure is 5.0Mpa, systemic circulation tolerance keeps 2000h
-1volume space velocity, H in system gas
2content accounts for 70%(volume fraction).
The method of operating of embodiment 3 one kinds of methyl alcohol catalyst heating reductions, comprises the following steps: (a) temperature rise period; Reaction system rises to 70 DEG C by room temperature, and catalyst stratification temperature difference is 0 DEG C, heating rate 15-20 DEG C/h, time 3.5h; (b) reduction phase initial stage; First stage, catalyst layer hot(test)-spot temperature rises to 80 DEG C by 70 DEG C, and catalyst stratification temperature differs from 5 DEG C, programming rate rate 0-5 DEG C/h, Chu Shui Liang≤2Kg/ ton catalyst/h, time 2.5h; Second stage, catalyst layer hot(test)-spot temperature rises to 95 DEG C by 80 DEG C, and catalyst stratification temperature differs from 12 DEG C, programming rate rate 0-1 DEG C/h, Chu Shui Liang≤4Kg/ ton catalyst/h, time 23h; C () is reduced the main phase; First stage, catalyst layer hot(test)-spot temperature rises to 120 DEG C by 95 DEG C, and catalyst stratification temperature differs from 7 DEG C, heating rate 1-3 DEG C/h, Chu Shui Liang≤3Kg/ ton catalyst/h, time 17h; Second stage, catalyst layer hot(test)-spot temperature rises to 140 DEG C by 120 DEG C, and catalyst stratification temperature differs from 5 DEG C, heating rate 0-1 DEG C/h, Chu Shui Liang≤4Kg/ ton catalyst/h, time 23h; Phase III, catalyst layer hot(test)-spot temperature rises to 160 DEG C by 140 DEG C, and catalyst stratification temperature differs from 3 DEG C, heating rate 1 ~ 3 DEG C/h, Chu Shui Liang≤3Kg/ ton catalyst/h, time 12h; D () is reduced latter stage; First stage, catalyst layer hot(test)-spot temperature rises to 200 DEG C by 160 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 3-10 DEG C/h, Chu Shui Liang≤2Kg/ ton catalyst/h, time 7h; Second stage, catalyst layer hot(test)-spot temperature rises to 240 DEG C by 200 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 10 DEG C/h, Chu Shui Liang≤1.5Kg/ ton catalyst/h, time 4h; (e) constant temperature stage; Temperature range is 240 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 0 DEG C/h, Chu Shui Liang≤2Kg/h, and the time keeps 2h.Above in each step, all require that keeping system pressure is 5.0Mpa, systemic circulation tolerance keeps 2000h
-1volume space velocity, H in system gas
2content with volume fraction calculating for 70%.
For above-mentioned each embodiment, when keeping system pressure and systemic circulation tolerance stable, heating rate speed in each stage should be adjusted according to water yield size, thus within the scope of each phases-time extend or shorten each heating reduction time in stage; For reduction initial stage second stage, namely catalyst layer hot(test)-spot temperature rises to 95 DEG C by 80 DEG C, and reduce main phase second stage and catalyst layer hot(test)-spot temperature and rise to 140 DEG C of these two stages by 120 DEG C, by keeping constant temperature and the mode combined that heats up, make water yield can not exceed this stage water yield requirement; Described systemic circulation tolerance refers to by volume flow 0.5m
3/ min/ ton catalyst.As risen in 95 DEG C of these temperature ranges for catalyst layer hot(test)-spot temperature by 80 DEG C, adopting constant temperature 0 DEG C and heating 1 DEG C of mode combined, and keeping water yield to maintain within the scope of regulation separately.
Reduction reaction process regulation principle: principle that reduction reaction is strictly followed " three low, three steady, three controls ", " three is low " i.e. low temperature water outlet, low pressure delivery and underrun a period of time, " three is steady " i.e. temperature is steady, pressure is steady, water yield is steady, " three controls " i.e. control temperature, control water yield, control CO
2% content.These conditions influence each other, therefore mainly keeping system pressure within 5.0 ± 0.1MPa, due to H in reduction reaction
2participate in reaction and be constantly consumed, in order to keep H in gas
2% content about 70%, needs with the elevated temperature gas pipeline of special preferably DN15 or DN20 be equipped with at 80 DEG C later and is system continuous supplementation sub-fraction live gas, realizes substitution gas and maintain the stable object of system pressure by emptying after tower.1m is coordinated according to practical experience 2 tons of catalyst
3the internal circulating load of/min, to be converted under 5.0MPa system pressure namely approximately 3000Nm
3/the internal circulating load of h, observe through using, this internal circulating load is moderate, 10 tons of general 15000Nm of catalyst
3/h internal circulating load, should keep inconvenience in whole reduction process.Like this at pressure, H
2when % content and internal circulating load remain unchanged, control heating rate well, ensure that the supply of temperature heat just can ensure that water yield is relatively stable, Gao Feng Qi≤3 ~ 5Kg/ ton catalyst/h in right amount, reduction reaction intensity stabilization is even, and catalyst just can be made to have good activity when forming active cells structure.Owing to containing CO in catalyst
3radical ion, therefore will discharge sub-fraction CO in reduction process
2gas, why Here it is arrives the reason that the reduction middle and later periods goes out water-band alcohol taste.If supplement containing ammonia in virgin gas, so water outlet will because of containing Cu (NH
3 ) 2+ion and aobvious blue, therefore avoids containing ammonia in gas as far as possible, in case copper run off (this kind of tonifying Qi mainly due to wash through copper refining after gas and containing Ammonia).
Because internal circulating load is large and obviously, therefore maintain stable to reduction reaction intensity effect as far as possible, otherwise strengthen, to reduce and water yield strengthens, reduces along with internal circulating load, be unfavorable for stable water outlet.In addition, due to go out mechanical water reaction be molecular diffusion control (under certain temperature conditions), therefore internal circulating load to 80 DEG C ~ 95 DEG C period water yield play controlled condition.The change of system pressure also directly affects the precipitation of water, therefore will make every effort to internal circulating load, system pressure is stablized.
Claims (2)
1. a method of operating for methyl alcohol catalyst heating reduction, comprises the following steps: (a) temperature rise period; Reaction system rises to 70 DEG C by room temperature, and catalyst stratification temperature difference is 0 DEG C, heating rate 15-20 DEG C/h, time 3 ~ 4h; (b) reduction phase initial stage; First stage, catalyst layer hot(test)-spot temperature rises to 80 DEG C by 70 DEG C, and catalyst stratification temperature differs from 5 DEG C, heating rate 0-5 DEG C/h, Chu Shui Liang≤1 ~ 3Kg/ ton catalyst/h, time 2 ~ 3h; Second stage, catalyst layer hot(test)-spot temperature rises to 95 DEG C by 80 DEG C, catalyst stratification temperature difference 10-15 DEG C, programming rate rate 0-1 DEG C/h, Chu Shui Liang≤3 ~ 5Kg/ ton catalyst/h, time 20 ~ 25h; C () is reduced the main phase; First stage, catalyst layer hot(test)-spot temperature rises to 120 DEG C by 95 DEG C, catalyst stratification temperature difference 5-10 DEG C, heating rate 1-3 DEG C/h, Chu Shui Liang≤2 ~ 4Kg/ ton catalyst/h, time 15 ~ 20h; Second stage, catalyst layer hot(test)-spot temperature rises to 140 DEG C by 120 DEG C, and catalyst stratification temperature differs from 5 DEG C, heating rate 0-1 DEG C/h, Chu Shui Liang≤3 ~ 5Kg/ ton catalyst/h, time 20 ~ 25h; Phase III, catalyst layer hot(test)-spot temperature rises to 160 DEG C by 140 DEG C, catalyst stratification temperature difference 0-5 DEG C, heating rate 1 ~ 3 DEG C/h, Chu Shui Liang≤2 ~ 4Kg/ ton catalyst/h, time 10 ~ 15h; D () is reduced latter stage; First stage, catalyst layer hot(test)-spot temperature rises to 200 DEG C by 160 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 3-10 DEG C/h, Chu Shui Liang≤1 ~ 3Kg/ ton catalyst/h, time 5 ~ 10h; Second stage, catalyst layer hot(test)-spot temperature rises to 240 DEG C by 200 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 10 DEG C/h, Chu Shui Liang≤1 ~ 2Kg/ ton catalyst/h, time 4h; (e) constant temperature stage; Temperature range is 240 DEG C, and catalyst stratification temperature differs from 0 DEG C, heating rate 0 DEG C/h, Chu Shui Liang≤2Kg/h, and the time keeps 2h; First stage at reduction phase initial stage and second stage and the temperature-rise period of main phase second stage of reducing are one and heat up and the process of constant temperature dynamic bind, regulate heating rate size, ensure that water yield is no more than corresponding requirements by corresponding water yield; Above in each step, all require that keeping system pressure is 5.0MPa, systemic circulation tolerance keeps 2000h
-1volume space velocity, H in system gas
2content with volume fraction calculating for 70%.
2. the method for operating of a kind of methyl alcohol catalyst heating reduction as claimed in claim 1, it is characterized in that, when keeping system pressure and systemic circulation tolerance stable, heating rate speed in each stage should be adjusted according to water yield size, thus extend within the scope of each phases-time or shorten the heating reduction time; For reduction initial stage second stage, namely catalyst layer hot(test)-spot temperature rises to 95 DEG C by 80 DEG C, and reduce main phase second stage and catalyst layer hot(test)-spot temperature and rise to 140 DEG C of these two stages by 120 DEG C, should, by keeping constant temperature and the mode combined that heats up, make water yield can not exceed this stage water yield requirement; Described systemic circulation tolerance refers to by volume flow 0.5m
3/ min/ ton catalyst.
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