CN102649564A - Method for dehydrogenating CO-containing mixed gas raw material by means of catalytic oxidation reaction - Google Patents
Method for dehydrogenating CO-containing mixed gas raw material by means of catalytic oxidation reaction Download PDFInfo
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Abstract
The invention relates to a method for dehydrogenating a CO-containing mixed gas raw material by means of a catalytic oxidation reaction. According to the method, the technical problems of difficulty in temperature control, low hydrogen gas removing rate and high CO loss rate in the dehydrogenation process of the CO-containing mixed gas raw material by means of the catalytic oxidation reaction in the prior art are mainly solved. The technical scheme adopted by the invention is that the method is realized by the step that with gases containing hydrogen gas and CO as raw materials and under the conditions that the reaction temperature is 80-260DEG C, the volume space velocity is 100-10000 hour<-1>, the mole ratio of oxygen gas to hydrogen gas is (0.5-10):1 and the reaction pressure is -0.08MPa to 5.0MPa, the raw materials are sequentially contacted with noble metal catalysts in an upper heat-insulated catalyst bed, a heat exchange catalyst bed and a lower heat-insulated catalyst bed of an enhanced heat exchange combined reactor in a hot spot distribution area and the hydrogen gas in the raw materials is oxidized into water. According to the technical scheme, the problems are better solved. The method can be used for the industrial production of the dehydrogenation of the CO-containing mixed gas raw material by means of the catalytic oxidation reaction.
Description
Technical field
The present invention relates to the method for a kind of CO of containing mixed gas feed by the catalytic oxidation dehydrogenation; Particularly about adopting focus distributed areas enhanced heat exchange combined reactor; Realize that CO mixed gas feed catalytic oxidative dehydrogenation reacts, be useful for to contain in the CO mixed gas feed catalytic oxidative dehydrogenation reaction process.
Background technology
Barkite is important Organic Chemicals, is used for fine chemistry industry in a large number and produces various dyestuffs, medicine, important solvent, extraction agent and various midbody.Get into 21 century, barkite receives international extensively attention as degradable environment-friendly engineering plastics monomer.In addition, the barkite ordinary-pressure hydrolysis can get oxalic acid, and normal pressure ammonia is separated and can be got high-quality slow chemical fertilizer oxamyl.Barkite can also be used as solvent, produces medicine and dyestuff intermediate etc., for example carries out various condensation reactions with fatty ester, hexamethylene phenyl methyl ketone, amido alcohol and many heterogeneous ring compounds.It can also synthesize at the chest acyl alkali that pharmaceutically is used as hormone.In addition, the barkite low-voltage hydrogenation can prepare crucial industrial chemicals terepthaloyl moietie, and terepthaloyl moietie mainly relies on petroleum path to prepare at present, and cost is higher, and China needs a large amount of import terepthaloyl moietie every year, and import volume was nearly 4,800,000 tons in 2007.
The production route of tradition barkite utilizes oxalic acid to prepare with alcohol generation esterification, and the production technique cost is high, and energy consumption is big, and is seriously polluted, and prepared using is unreasonable.And adopt the carbon monoxide coupling technology to produce the focus that barkite has become domestic and international research.
As everyone knows; Carbon monoxide can be from the various gas mixtures that contain carbon monoxide separation and Extraction, the virgin gas that can be used for separating carbon monoxide in the industry comprises: the tail gas of synthetic gas, water-gas, semi-water gas and Iron And Steel Plant, calcium carbide factory and yellow phosphorus factory that Sweet natural gas and oil transform etc.It is pressure swing adsorption process that existing CO separates the main method of purifying; China has many companies to develop transformation fractionation by adsorption carbon monoxide new technology; Especially the high-efficiency adsorbent of developing; Carbon monoxide there are high loading capacity and selectivity, can solve a difficult problem of from the high virgin gas of nitrogen or methane content, isolating high-purity carbon monooxide, can design and build up large-scale carbon monoxide tripping device.However, by this technology isolated carbon monoxide from synthetic gas, under the prerequisite of taking into account the carbon monoxide yield, generally the content of its hydrogen can reach more than 1%.And research shows that the existence of hydrogen can cause the active reduction of follow-up CO coupling reaction catalyst, can't carry out until reaction, and therefore, the exploitation carbon monoxide selects the dehydrogenation technical meaning great.
At present, the dehydrogenation catalyst of report mainly contains Pd/Al both at home and abroad
2O
3, CoMo/Al
2O
3Deng, the dehydrogenating agent based on the manganese series metal oxide is also arranged, but generally being used for the dehydrogenation of non-reducing gas such as high purity nitrogen, high purity oxygen and carbonic acid gas, these catalyzer or dehydrogenating agent purify.And exist down for the CO reducing gas, catalyzer is low to the decreasing ratio of hydrogen, and the rate of loss of CO is high.As adopt the method and the catalyzer of the disclosed catalytic oxidative dehydrogenation of document CN97191805.8, and be raw material at the CO mixed gas that is used for hydrogen content 10%, 220 ℃ of temperature of reaction, volume space velocity 3000 hours
-1, oxygen/hydrogen mol ratio is 0.6: 1, and reaction pressure is under the condition of 0.5MPa, and the rate of loss of CO is up to 1.5%, and the content of hydrogen is up to 1000ppm in the reaction effluent.
The subject matter that the related technology of above-mentioned document exists is that technology and catalyzer are unreasonable, causes the carbon monoxide rate of loss high, and hydrogen removes not thorough.
Summary of the invention
Technical problem to be solved by this invention is to be used for containing the CO mixed gas feed by the catalytic oxidation dehydrogenation reaction process in the technical literature in the past; Temperature control difficulty; Exist the hydrogen decreasing ratio low; The technical problem that the CO rate of loss is high provides a kind of new method of CO mixed gas feed by the catalytic oxidation dehydrogenation that contain.This contains the CO mixed gas feed, and dehydrogenation is used for containing CO mixed gas feed catalytic oxidative dehydrogenation process by catalytic oxidation, and temperature control evenly has hydrogen decreasing ratio height, the advantage that the CO rate of loss is low.
In order to solve the problems of the technologies described above; The technical scheme that the present invention adopts is following: a kind of method that contains the CO mixed gas feed by the catalytic oxidation dehydrogenation; Gas with hydrogen and CO is raw material, is 80～260 ℃ in temperature of reaction, and volume space velocity is 100～10000 hours
-1Oxygen/hydrogen mol ratio is 0.5～10: 1; Reaction pressure is under the condition of-0.08～5.0MPa; Raw material successively with focus distributed areas enhanced heat exchange combined reactor in last adiabatic catalyst beds, heat exchange catalyst bed and following adiabatic catalyst beds in noble metal catalyst contact; Hydrogen in the raw material is oxidized to water, and wherein enhanced heat exchange combined reactor in focus distributed areas is made up of feed(raw material)inlet (1), porous gas grid distributor (3), gas distribution chamber (4), last adiabatic catalyst beds (5), heat exchange catalyst bed (6), following adiabatic catalyst beds (7), heat transfer tube (13), collection chamber (8) and porous gas collection plate (9) basically, is primarily characterized in that heat exchange catalyst bed (6) is positioned at the bottom of adiabatic catalyst beds (5); The top of following adiabatic catalyst beds (7), and heat transfer tube (13) is set in the heat exchange catalyst bed (6).
Porous gas collection plate (9) is positioned at collection chamber (8) in the technique scheme, and is connected with pneumatic outlet (10).Porous gas grid distributor (3) is positioned at gas distribution chamber (4), and is connected with feed(raw material)inlet (1).Last adiabatic catalyst beds (5) top is 1/30～1/6 of reactor length apart from the length of porous gas grid distributor (3) bottom; The bottom of following adiabatic catalyst beds (7) is 1/30～1/6 of a height for reactor apart from the vertical height on porous gas collection plate (9) top.The height of last adiabatic catalyst beds (5) is 1/6～3/2 of heat exchange catalyst bed (a 6) height, and following adiabatic catalyst beds (7) is 1/6～1/1 of heat exchange catalyst bed (a 6) height.
Reaction conditions is preferably in the technique scheme: temperature of reaction is 120～240 ℃, and volume space velocity is 500～6000 hours
-1, oxygen/hydrogen mol ratio is 0.5～4: 1, and reaction pressure is 0.01～2.0MPa, and the noble metal catalyst active ingredient is preferably selected from palladium or platinum, and carrier is preferably selected from aluminum oxide.
As everyone knows, the reaction of hydrogen and oxygen is high-intensity thermopositive reaction, and the hydrogen in the presence of CO removes reaction, requires very high to temperature controlling.If temperature control is improper, may cause because of temperature drift and cause CO and oxygen reaction, this not only can cause thermal discharge further to strengthen; Temperature further raises; And the loss of CO also can sharply increase, and it is most important through the oxidative dehydrogenation process to containing the CO gaseous mixture therefore to control the reaction bed uniformity of temperature profile, and the temperature distribution of beds is even more; The selection of hydrogen just removes control more easily, and keeps lower CO rate of loss easily.For the fixed-bed reactor of routine, because catalyzed reaction is carried out on catalyzer and not according to front and back phase uniform velocity, general reactor drum is anterior from balanced remote; Speed of response is fast, and it is also many to emit reaction heat, shows as anterior mid-way partially and occurs significant hot spot region easily; And the rear portion with reaction near balance, speed of response slows down, it is also few to emit reaction heat; If adopt conventional shell-and-tube reactor, the same before and after the temperature of its refrigerant, if reduce coolant temperature like this; Strengthen heat transfer temperature difference and move heat; Reach the heat request that moves of high speed of response of middle front part and strong reaction heat, then reactor lower part or rear portion reaction heat reduce, and move heat and cause temperature of reaction to descend greater than reaction heat; Speed of response is further slowed down below catalyst activity with regard to stopped reaction, therefore be difficult to the way that makes the best of both worlds of accomplishing that the front and rear part reaction is all carried out under optimal reaction temperature.The present invention is directed to this fundamental contradiction, and, heat transfer zone is set at the reactor drum middle part according to the characteristic exotherm that reacts; And the reactor drum two ends are provided with adiabatic region, make the hot spot region flattening, and temperature distribution more becomes evenly rationally; This is for the efficient of maximized performance catalyzer; Farthest reduce the loss of CO, and remove the hydrogen in the raw material comparatively up hill and dale, useful effect is provided.
The present invention uses device shown in Figure 1, focus distributed areas enhanced heat exchange combined reactor, and accurate controlled temperature, adopting precious metal palladium or platinum load aluminum oxide is catalyzer, is 80～260 ℃ in temperature of reaction, volume space velocity is 100～10000 hours
-1Oxygen/hydrogen mol ratio is 0.5～10: 1, and reaction pressure is under the condition of-0.08～5.0MPa, raw material successively with focus distributed areas enhanced heat exchange combined reactor in last adiabatic catalyst beds, heat exchange catalyst bed and following adiabatic catalyst beds in noble metal catalyst contact; Hydrogen in the raw material is oxidized to water; In containing the gas raw material of CO, the volumn concentration of hydrogen is that the decreasing ratio of hydrogen can reach 100% greater than under 0～15% the condition; The rate of loss of CO can obtain better technical effect less than 0.3%.
Description of drawings
The focus distributed areas enhanced heat exchange combined reactor synoptic diagram that Fig. 1 adopts for the present invention.
1 is the feed(raw material)inlet among Fig. 1, the 2nd, and manhole, the 3rd, porous gas grid distributor, the 4th, gas distribution chamber; The 5th, last adiabatic catalyst beds, the 6th, heat exchange catalyst bed, the 7th, following adiabatic catalyst beds, the 8th, collection chamber; The 9th, porous gas collection plate, the 10th, pneumatic outlet, the 11st, catalyzer unloads outlet, and the 12nd, the heat transferring medium outlet; The 13rd, heat transfer tube, the 14th, heat transferring medium inlet, the 15th, reactor drum tank body.
Raw material is introduced by feed(raw material)inlet 1 among Fig. 1; Gas gets into distributing chamber's 4 further mixed distribution after porous gas grid distributor 3 distributes; Get into then and go up adiabatic catalyst beds 5 and catalyzer contact reacts, have the reaction effluent of certain temperature rise to get into heat exchange catalyst bed 6 again, the heat that discharges in the reaction process carries out shifting out of heat through heat transfer tube 13; Keep the temperature in the heat exchange catalyst bed 6 even; After adiabatic catalyst beds 7 further reacted completely under the last entering of elute behind most of raw material reaction, elute got into collection chamber 8, gets into follow-up system through porous gas collection plate 9 through pneumatic outlet 10.Because the hot(test)-spot temperature distributed areas adopt heat transfer tube to carry out shifting out and controlling of heat, thereby reach the effect that the whole reactor catalyst bed temperature is uniformly distributed with.
Through embodiment the present invention is done further elaboration below.
Embodiment
[embodiment 1]
Focus distributed areas enhanced heat exchange combined reactor with Fig. 1; Adopt the catalyzer in the heat transfer tube heat exchanging catalyst bed to carry out heat exchange; Wherein, the last adiabatic catalyst beds top of reactor drum is 1/20 of reactor length apart from the length of porous gas grid distributor bottom; The bottom of following adiabatic catalyst beds is 1/10 of a height for reactor apart from the vertical height on porous gas collection plate top; The height of the last adiabatic catalyst beds of reactor drum is 1/8 of a heat exchange catalyst bed height; Following adiabatic catalyst beds is 1/4 of a heat exchange catalyst bed height, is that the catalyzer of 0.5% palladium load aluminum oxide is a catalyzer with palladium content, uses the CO mixed gas of hydrogen content 10% to be raw material; At 220 ℃ of reaction temperature ins, volume space velocity 3000 hours
-1, oxygen/hydrogen mol ratio is 0.6: 1, and reaction pressure is under the condition of 0.5MPa, and reaction result is: the rate of loss of CO is 0.32%, and the content of hydrogen is 0ppm in the reaction effluent, reactor catalyst bed temperature difference is less than 10 ℃.
[embodiment 2]
Focus distributed areas enhanced heat exchange combined reactor with Fig. 1; Adopt the catalyzer in the heat transfer tube heat exchanging catalyst bed to carry out heat exchange; Wherein, the last adiabatic catalyst beds top of reactor drum is 1/10 of reactor length apart from the length of porous gas grid distributor bottom; The bottom of following adiabatic catalyst beds is 1/20 of a height for reactor apart from the vertical height on porous gas collection plate top; The height of the last adiabatic catalyst beds of reactor drum is 1/3 of a heat exchange catalyst bed height; Following adiabatic catalyst beds is 1/4 of a heat exchange catalyst bed height, is that the catalyzer of 0.2% palladium load aluminum oxide is a catalyzer with palladium content, uses the CO mixed gas of hydrogen content 5% to be raw material; At 200 ℃ of reaction temperature ins, volume space velocity 1000 hours
-1, oxygen/hydrogen mol ratio is 0.7: 1, and reaction pressure is under the condition of 0.1MPa, and reaction result is: the rate of loss of CO is 0.15%, and the content of hydrogen is 3ppm in the reaction effluent, reactor catalyst bed temperature difference is less than 8 ℃.
[embodiment 3]
With the focus distributed areas enhanced heat exchange combined reactor of Fig. 1, adopt the catalyzer in the heat transfer tube heat exchanging catalyst bed to carry out heat exchange, wherein, the last adiabatic catalyst beds top of reactor drum is 1/8 of reactor length apart from the length of porous gas grid distributor bottom; The bottom of following adiabatic catalyst beds is 1/5 of a height for reactor apart from the vertical height on porous gas collection plate top; The height of the last adiabatic catalyst beds of reactor drum is 1/3 of a heat exchange catalyst bed height; Following adiabatic catalyst beds is 1/6 of a heat exchange catalyst bed height, is that the catalyzer of 0.3% palladium load aluminum oxide is a catalyzer with palladium content, uses the CO mixed gas of hydrogen content 1% to be raw material; At 180 ℃ of reaction temperature ins, volume space velocity 5000 hours
-1, oxygen/hydrogen mol ratio is 0.8: 1, and reaction pressure is under the condition of 2.5MPa, and reaction result is: the rate of loss of CO is 0.15%, and the content of hydrogen is 3ppm in the reaction effluent, reactor catalyst bed temperature difference is less than 6 ℃.
[embodiment 4]
Focus distributed areas enhanced heat exchange combined reactor with Fig. 1; Adopt the catalyzer in the heat transfer tube heat exchanging catalyst bed to carry out heat exchange; Wherein, the last adiabatic catalyst beds top of reactor drum is 1/15 of reactor length apart from the length of porous gas grid distributor bottom; The bottom of following adiabatic catalyst beds is 1/20 of a height for reactor apart from the vertical height on porous gas collection plate top; The height of the last adiabatic catalyst beds of reactor drum is 1/3 of a heat exchange catalyst bed height; Following adiabatic catalyst beds is 1/4 of a heat exchange catalyst bed height, is that the catalyzer of 0.2% palladium load aluminum oxide is a catalyzer with palladium content, uses the CO mixed gas of hydrogen content 0.5% to be raw material; At 180 ℃ of reaction temperature ins, volume space velocity 4000 hours
-1, oxygen/hydrogen mol ratio is 0.6: 1, reaction pressure is-condition of 0.05MPa under, reaction result is: the rate of loss of CO is 0.11%, the content of hydrogen is 1ppm in the reaction effluent, reactor catalyst bed temperature difference is less than 5 ℃.
[embodiment 5]
With the focus distributed areas enhanced heat exchange combined reactor of Fig. 1, adopt the catalyzer in the heat transfer tube heat exchanging catalyst bed to carry out heat exchange, wherein, the last adiabatic catalyst beds top of reactor drum is 1/8 of reactor length apart from the length of porous gas grid distributor bottom; The bottom of following adiabatic catalyst beds is 1/20 of a height for reactor apart from the vertical height on porous gas collection plate top; The height of the last adiabatic catalyst beds of reactor drum is 1/2 of a heat exchange catalyst bed height; Following adiabatic catalyst beds is 1/3 of a heat exchange catalyst bed height, is that the catalyzer of 0.1% platinum load aluminum oxide is a catalyzer with platinum content, uses the CO mixed gas of hydrogen content 0.8% to be raw material; At 260 ℃ of reaction temperature ins, volume space velocity 500 hours
-1, oxygen/hydrogen mol ratio is 0.7: 1, and reaction pressure is under the condition of 0.01MPa, and reaction result is: the rate of loss of CO is 0.16%, and the content of hydrogen is 3ppm in the reaction effluent, reactor catalyst bed temperature difference is less than 5 ℃.
[comparative example 1]
Each step and reaction conditions with reference to embodiment 1; Just contain CO mixed gas feed catalytic oxidative dehydrogenation reactor drum and adopt insulation fix bed reactor; Reaction result is: the rate of loss of CO is 3.2%, and the content of hydrogen is 160ppm in the reaction effluent, and reactor catalyst bed temperature difference is 18 ℃.
[comparative example 2]
Each step and reaction conditions with reference to embodiment 2; Just CO mixed gas feed catalytic oxidative dehydrogenation reactor drum adopts insulation fix bed reactor; Reaction result is: the rate of loss of CO is 4.2%, and the content of hydrogen is 180ppm in the reaction effluent, and reactor catalyst bed temperature difference is 12 ℃.
Claims (6)
1. method that contains the CO mixed gas feed by the catalytic oxidation dehydrogenation is a raw material with the gas of hydrogen and CO, is 80～260 ℃ in temperature of reaction, and volume space velocity is 100～10000 hours
-1Oxygen/hydrogen mol ratio is 0.5～10: 1; Reaction pressure is under the condition of-0.08～5.0MPa; Raw material successively with focus distributed areas enhanced heat exchange combined reactor in last adiabatic catalyst beds, heat exchange catalyst bed and following adiabatic catalyst beds in noble metal catalyst contact; Hydrogen in the raw material is oxidized to water, and wherein enhanced heat exchange combined reactor in focus distributed areas is made up of feed(raw material)inlet (1), porous gas grid distributor (3), gas distribution chamber (4), last adiabatic catalyst beds (5), heat exchange catalyst bed (6), following adiabatic catalyst beds (7), heat transfer tube (13), collection chamber (8) and porous gas collection plate (9) basically, is primarily characterized in that heat exchange catalyst bed (6) is positioned at the bottom of adiabatic catalyst beds (5); The top of following adiabatic catalyst beds (7), and heat transfer tube (13) is set in the heat exchange catalyst bed (6).
2. according to the said method that contains the CO mixed gas feed by the catalytic oxidation dehydrogenation of claim 1, it is characterized in that the porous gas collection plate (9) of reactor drum is positioned at collection chamber (8), and be connected with pneumatic outlet (10).
3. according to the said method that contains the CO mixed gas feed by the catalytic oxidation dehydrogenation of claim 1, it is characterized in that the porous gas grid distributor (3) of reactor drum is positioned at gas distribution chamber (4), and be connected with feed(raw material)inlet (1).
4. according to the said method that contains the CO mixed gas feed by the catalytic oxidation dehydrogenation of claim 1, last adiabatic catalyst beds (5) top that it is characterized in that reactor drum is 1/30～1/6 of reactor length apart from the length of porous gas grid distributor (3) bottom; The bottom of following adiabatic catalyst beds (7) is 1/30～1/6 of a height for reactor apart from the vertical height on porous gas collection plate (9) top.
5. according to the said method that contains the CO mixed gas feed by the catalytic oxidation dehydrogenation of claim 1; The height that it is characterized in that the last adiabatic catalyst beds (5) of reactor drum is 1/6～3/2 of heat exchange catalyst bed (a 6) height, and following adiabatic catalyst beds (7) is 1/6～1/1 of heat exchange catalyst bed (a 6) height.
6. according to the said method that contains the CO mixed gas feed by the catalytic oxidation dehydrogenation of claim 1, it is characterized in that temperature of reaction is 120～240 ℃, volume space velocity is 500～6000 hours
-1, oxygen/hydrogen mol ratio is 0.5～4: 1, and reaction pressure is 0.01～2.0MPa, and the noble metal catalyst active ingredient is selected from palladium or platinum, and carrier is selected from aluminum oxide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018096018A1 (en) * | 2016-11-24 | 2018-05-31 | Haldor Topsøe A/S | Multi bed reactor comprising an adiabatic and a heated catalyst bed |
| CN110841563A (en) * | 2019-11-27 | 2020-02-28 | 云南电网有限责任公司电力科学研究院 | Device and method for dehydrogenation by utilizing tail gas of thermomotor |
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| JPS5688801A (en) * | 1979-10-27 | 1981-07-18 | Mitsubishi Gas Chem Co Inc | Separating and obtaining method of hydrogen and carbon monoxide |
| JP2003144924A (en) * | 2001-11-09 | 2003-05-20 | Mitsubishi Chemicals Corp | Selective oxidation catalyst for hydrogen, selective oxidation method for hydrogen and dehydrogenation method for hydrocarbon |
| CN2621805Y (en) * | 2003-06-03 | 2004-06-30 | 华东理工大学 | Shell external cooling-thermal insulating and combined fixed bed catalyst chember |
| CN101543776A (en) * | 2009-04-28 | 2009-09-30 | 华烁科技股份有限公司 | Dehydrogenation catalyst for feed gas containing carbon monoxide, preparation method and application method thereof |
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2011
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5688801A (en) * | 1979-10-27 | 1981-07-18 | Mitsubishi Gas Chem Co Inc | Separating and obtaining method of hydrogen and carbon monoxide |
| JP2003144924A (en) * | 2001-11-09 | 2003-05-20 | Mitsubishi Chemicals Corp | Selective oxidation catalyst for hydrogen, selective oxidation method for hydrogen and dehydrogenation method for hydrocarbon |
| CN2621805Y (en) * | 2003-06-03 | 2004-06-30 | 华东理工大学 | Shell external cooling-thermal insulating and combined fixed bed catalyst chember |
| CN101543776A (en) * | 2009-04-28 | 2009-09-30 | 华烁科技股份有限公司 | Dehydrogenation catalyst for feed gas containing carbon monoxide, preparation method and application method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018096018A1 (en) * | 2016-11-24 | 2018-05-31 | Haldor Topsøe A/S | Multi bed reactor comprising an adiabatic and a heated catalyst bed |
| CN110841563A (en) * | 2019-11-27 | 2020-02-28 | 云南电网有限责任公司电力科学研究院 | Device and method for dehydrogenation by utilizing tail gas of thermomotor |
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