CN101491752B - Endothermic reaction method - Google Patents
Endothermic reaction method Download PDFInfo
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- CN101491752B CN101491752B CN2008100329314A CN200810032931A CN101491752B CN 101491752 B CN101491752 B CN 101491752B CN 2008100329314 A CN2008100329314 A CN 2008100329314A CN 200810032931 A CN200810032931 A CN 200810032931A CN 101491752 B CN101491752 B CN 101491752B
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Abstract
The invention relates to a method for heat absorbing reaction, and mainly solves the problems of large axial-radial temperature difference of a tubular fixed bed reactor using molten salt as a heat carrier, larger vibration of a reaction tube, and inconvenience to detach a catalyst in the prior art. The invention adopts the technical proposal that a heating tube is arranged in a reactor shell and a convex shoulder and conical spring structure is designed in the reaction tube, the method solves the problems well, and can be used for industrial production of the heat absorbing reaction.
Description
Technical field
The present invention relates to a kind of method of chemical reaction, relate in particular to a kind of method that is used for the endothermic reaction.
Background technology
Calandria type fixed bed reactor is widely used in the gas-solid-phase catalytic reaction process in chemical industry and the petrochemical industry industry, is one of chemical industry common equipment.General chemical reaction occurs in the reaction tube of filling catalyst, course of reaction is followed neither endothermic nor exothermic more, promptly at the tube side of reactor and shell side often with the exchange of heat, therefore reaction heat must be supplied with or shifted out by reaction body or thermophore timely and effectively, to guarantee the temperature equalization and temperature runaway and the coking of avoiding catalyst between reaction tube.So the quality of reactor heat exchange effect will directly influence reactivity worth, thereby influence the yield of conversion of raw material and product.
For the endothermic reaction of reaction temperature higher (usually more than 350 ℃), adopt the thermophore of fused salt usually as calandria type fixed bed reactor.Method commonly used is: fused salt at first heats outside reactor shell, promptly the bottom from reactor enters the reactor shell side after being heated to uniform temperature, fused salt after the heat exchange shifts out from the top of reactor shell side, and this fused salt must depend on pump for liquid salts in the realization of the external cyclic process of reactor enclosure.Because the permeability of fused salt is extremely strong; and there is certain corrosivity; when temperature surpasses 454 ℃; slight decomposition can take place in fused salt; its corrosivity increases with the rising of temperature in the presence of air; so fused salt is also answered blanketing with inert gas when using more than 454 ℃, this has proposed higher requirement just for the annexes such as pump for liquid salts, pipeline and valve of the fused salt circulatory system.
Producing ethylene from dehydration of ethanol is a typical endothermic reaction, and its main chemical equation is as follows:
This is reflected in the calandria type fixed bed reactor and finishes, and by the fused salt heat supply.Present common method is: in the external cover fused salt circulatory system of setting up of reactor enclosure, to provide reaction required heat.Concrete grammar is: the reactor lower part housing radially offer 1～2 fused salt inlet, radially offer 1～2 fused salt outlet in the reactor upper body; In the external outfit of reactor enclosure one cover high-temperature molten salt system, this system comprises at least: 1 basin that can hold all salt, pump for liquid salts, a cover heater, and the pipeline that matches, valve, liquid level meter etc.Solid-state fused salt in basin is heated to molten state with heater, and it is temperature required to be warmed up to reaction, delivers in the reactor shell with pump for liquid salts then, the supply response heat, and the fused salt after the cooling flows back to basin.The shortcoming of this method is: 1. because fused salt mobile relatively poor, heat transfer coefficient is less, and the limited amount (one or two) of the fused salt inlet/outlet on reactor shell, when device is driven, high-temperature molten salt is difficult to reach at short notice even distribution, cause the diameter of axle in the shell side of reactor to the temperature distribution inequality, therefore be difficult to guarantee full and uniform heat transmission between reaction tube, and the reaction speed of most heterogeneous catalytic reaction is fast, it is strong suction (putting) thermal process, heat must be supplied with or remove by reacting gas and thermophore (as fused salt) timely and effectively, and is even to temperature with the diameter of axle that guarantees the thermophore between reaction tube.Reaction at above producing ethylene from dehydration of ethanol, in case temperature is on the low side, can cause ethanol conversion to reduce, and help intermolecular dehydration and generate the accessory substance ether, but temperature is too high, not only can cause the catalyst carbon deposit inactivation, shortens the life cycle of catalyst, also increase simultaneously the growing amount of alcohol dehydrogenase product-acetaldehyde, had a strong impact on product quality.2. because the outer circulation fused salt has big kinetic energy when entering reactor shell, and near the reaction tube the fused salt charge door is compared with other reaction tube, be subjected to the impact of bigger high-temperature molten salt and the tube vibration that induces reaction.3. fused salt circulatory system more complicated, especially quite high to the requirement of pump for liquid salts, often need import, increased the cost of device virtually, and the design of the fused salt circulatory system has also accounted for a greater part of of reaction system, and the quality of this system's operation often plays conclusive effect.
A kind of calandria type fixed bed reactor is disclosed among the Chinese patent CN2443770Y, this reactor is provided with a circle by fused salt outlet thereon and following fused salt porch and goes up circular passage under a circular passage and the circle outside the circumference of wall of reactor, and it is wide, equidistantly but not contour bar hole to be provided with a circle on the circular passage, the height in hole flows to from the extremely low tactic technical scheme of height along fused salt, and radially the temperature difference is as much as possible little with thermophore between the assurance reaction tube.But this method for designing requirement distributes to the fluidised form of thermophore in the circular passage and makes accurate Calculation, thereby determines bore size; And the manufacturing of reactor there is higher requirement.
In addition, calandria type fixed bed reactor is walked material at its tube side often, therefore filling catalyst in the reaction tube of reactor leaks from the lower end of pipe in order to prevent catalyst, and the structure of reaction tube lower end adopts pipe cap structure and spring to add the structure of baffle plate usually.Pipe cap structure wherein is meant, processes a pipe cap, and metal screen is set in the pipe cap, and pipe cap and pipe adopt and be threaded or bayonet coupling.When being threaded, need pipe cap upper end machining internal thread at reaction tube lower end threading.During bayonet coupling, need, correspondingly on pipe cap open two L shaped notches, earlier the notch of pipe cap is aimed at during installation on the fixture block of reaction tube lower end and pushed away, with angle of pipe cap rotation, pipe cap is clamped on the reaction tube pipe end then at two fixture blocks of reaction tube lower end weldering.Shortcoming is: 1. the pipe cap structure is occupied certain space, and the centre-to-centre spacing of reaction tube is strengthened, and causes reactor volume to strengthen, and is unfavorable for conducting heat; 2. after passing through long high-temperature operation, being threaded is difficult to dismounting, easily causes the damage of reaction tube; 3. the pipe cap structure all need be processed pipe cap, and wire netting is set, and machined is carried out in the lower end of reaction tube, and the quantity of reactor internal reaction tubulation is often bigger, and just processing has increased workload, the also corresponding increase of expense to equipment for this.Spring wherein adds baffle arrangement and is meant, process a spring, stretch into the reaction tube lower end, and some baffle plates are set at the back side of the reactor lower perforated plate that is connected with reaction tube, offer the circular hole corresponding on the baffle plate with the reaction tube mouth of pipe, this Circularhole diameter must come off in reaction tube to prevent spring, and this baffle plate be fixed on the tube sheet by screw less than tube inner diameter.Shortcoming is: 1. need the baffle plate of processing belt perforate, and to reactor lower perforated plate processing screw counter bore, the thickness of tube sheet is increased to some extent, for the perforate and the reaction tube mouth of pipe that guarantees baffle plate is corresponding one by one, its requirement on machining accuracy is higher; 3. baffle plate belongs to tube sheet and is threaded, and is the same with being threaded of above-mentioned pipe cap structure, and through after the long high-temperature operation, being threaded is difficult to dismounting, makes troubles for the dismounting of reaction tube inner catalyst.
Summary of the invention
The technical problem that the present invention mainly solves is that thermophore (fused salt) system configuration that is used for the calandria type fixed bed reactor of the endothermic reaction in the prior art is loaded down with trivial details, involve great expense, and the diameter of axle in the reactor shell side is to the temperature distribution inequality, be difficult to guarantee full and uniform heat transmission between reaction tube, thereby influence the control of reaction temperature; It is serious that inside reactor divides reaction tube impacted by high-temperature molten salt, and the problem of the bigger vibration of pipe that induces reaction provides a kind of new method that is used for the endothermic reaction.This method has the structure of reactor compactness, and the diameter of axle is to having a narrow range of temperature, the characteristics that operate steadily.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method that is used for the endothermic reaction, reaction raw materials is contacted with catalyst in the calandria type fixed bed reactor reaction tube, reaction reaction of formation product, wherein raw material is selected from ethanol, butanediol, urea or formamide, described reactor comprises the feed(raw material)inlet, reactor shell, last lower perforated plate, reaction tube, reacting product outlet, it is characterized in that being provided with in the reactor at least two heating tubes stretches in the fused salt, be used to heat fused salt, fused salt is positioned at reactor shell, outside the reaction tube.
In the technique scheme, the preferred version of heating tube is evenly distributed for the circumferencial direction along reactor shell.The preferred version that heating tube is provided with the position is that heating tube is in the axial insertion housing of reactor upper body or in the axial insertion housing of reactor lower part housing or respectively in the axial insertion housing of reactor upper and lower housing.On the lower perforated plate that is positioned at reactor bottom of the electrically heated rod in the heating tube, topmost be positioned under the upper perforated plate of reactor.The reaction tube preferred version is that the lower end is provided with convex shoulder, and volute spring is set on the convex shoulder.The preferable range of convex shoulder quantity is 2～6, and evenly distributes along reaction tube tube wall circumferencial direction.The preferred version of volute spring is an interference fit for the internal diameter of its big end external diameter and reaction tube, and more preferably scheme is that the difference of the internal diameter of the big end external diameter of volute spring and reaction tube is 1～6mm.
In the technique scheme, interference fit refers to the internal diameter of the big end external diameter of volute spring greater than reaction tube.Convex shoulder can be made of smooth bar, and fixing with the tube wall welding of reaction tube, can not cause damage to reaction tube.During the dismounting catalyst,, spring can be laid down as long as volute spring is torqued-up to big end external diameter less than the convex shoulder internal diameter in the reaction tube tube wall.
Use the reactor after improving among the present invention, heating tube places in the reactor shell, be integral with set of reactors, constitute the version of inner Natural Circulation, both kept the original advantage of calandria type fixed bed reactor, can save again, made the structure of reactor compactness in the external cover fused salt circulatory system of setting up of reactor enclosure, save equipment investment greatly, simplified the reactor operating process.The electrically heated rod that is provided with in the heating tube can heat fused salt simultaneously, has avoided because fused salt mobile relatively poor, and heat transfer coefficient is less, very difficultly reaches even distribution at short notice, and causes the diameter of axle in the reactor shell side to the temperature distribution inequality.When device is driven, with traditional thermophore high-temperature molten salt by offering on the reactor shell 1～2 radially the fused salt inlet reactor that enters housing compare, reactor temperature of molten salt of the present invention is evenly distributed, less along the diameter of axle to the temperature difference, the heat exchange effect is better between reaction tube, has guaranteed that reaction reaches higher feed stock conversion and product yield.Secondly, the version of inner Natural Circulation can effectively be avoided because the outer loop high-temperature molten salt has big kinetic energy when entering reactor shell, impact and near the reaction tube the reactor shell fused salt inlet/outlet produced, thus the vibration of the tubulation that induces reaction.In the tube wall of reaction tube lower end volute spring is set, both can have kept the catalyst in the reaction tube not leak, reacting gas is passed through smoothly.Convex shoulder adds the structure of volute spring, neither occupies the space, has made things convenient for the dismounting of reaction tube inner catalyst again, has obtained better technical effect.
Description of drawings
Fig. 1 is the structural representation of calandria type fixed bed reactor.
Fig. 2 is the enlarged drawing of node I among Fig. 1.
In Fig. 1,1 is the feed(raw material)inlet, and 2 is upper perforated plate, 3 is heating tube, and 4 is electrically heated rod, and 5 is reaction tube, 6 is reactor shell, and 7 is tasty and refreshing for putting, and 8 is lower perforated plate, 9 is reacting product outlet, 10 is radial temperature meter mouth, and 11 is the porcelain circle, and 12 is catalyst, 13 is axial temperature meter mouth, and 14 is the fused salt charge door.
In Fig. 2,15 is volute spring, and 16 is convex shoulder.
Among Fig. 1, reaction raw materials enters the reactor reaction tubulation 5 from feed(raw material)inlet 1, contacts with the catalyst 12 of wherein filling, and the product that reaction obtains flows out from reacting product outlet 9.Reaction institute calorific requirement is provided by the fused salt that is positioned at reactor shell 6 inside, reaction tube 5 outsides, heats by 4 pairs of fused salts of the electrically heated rod in the heating tube 3.
The invention will be further elaborated below by embodiment.
The specific embodiment
[embodiment 1]
6000 tons of/year producing ethylene from dehydration of ethanol devices are raw material with ethanol, adopt calandria type fixed bed reactor shown in Figure 1, adopt aluminium oxide catalyst.The shell side temperature is 450 ℃, and the tube side temperature is 430 ℃, and reaction pressure is a normal pressure, and the raw material air speed is 1.0 hours
-1The reactor shell diameter is 1600 millimeters, the fused salt charge door is positioned at the axial of reactor upper body, 89 millimeters of heating tube external diameters, in the axial insertion housing of reactor upper body, being concentric circles in cylindrical shell evenly distributes, the number of the convex shoulder in 52 millimeters of the big end external diameters of 57 millimeters of reaction tube external diameters, volute spring, the tube wall of reaction tube lower end is 4, and evenly distributes along the tube wall circumferencial direction.900 millimeters places along the circumferential direction evenly are provided with 4 radial temperature meters at the reactor interior diameter, highly locate to be provided with respectively 2 thermometers in the axial distance reactor lower end 1/3 and 2/3 of reactor.Record 4 radial temperatures and be respectively 427.5 ℃, 428.3 ℃, 429.1 ℃ and 428.6 ℃; Record 2 axial temperatures and be respectively 426.3 ℃ and 427.6 ℃.Equipment operates steadily, and ethanol conversion is 99.5%, and selectivity of ethylene is 97.0%.
[comparative example 1]
The process conditions of certain producing ethylene from dehydration of ethanol device are all identical with embodiment 1 with the structure of reactor parameter, difference is, do not establish heating tube in the reactor, the external cover fused salt circulatory system of setting up of reactor enclosure, the fused salt inlet is positioned at the reactor lower part housing radially, and the fused salt outlet of increase is positioned at the reactor upper body radially; The pipe cap structure is adopted in the reaction tube lower end, and pipe cap and pipe adopt and be threaded.Adopt and arrange, record 4 radial temperatures and be respectively 425.5 ℃, 428.8 ℃, 431.5 ℃ and 424.2 ℃ as embodiment 1 described thermometer test point; Record 2 axial temperatures and be respectively 422.3 ℃ and 428.6 ℃.The equipment operation is less than half a year, leaking appears in the fused salt circulatory system, reaction temperature occurs than great fluctuation process, reactivity worth to catalyst in reactor exerts a certain influence, the connecting thread of the pipe cap of reaction tube and pipe occurs stuck in addition, be difficult to dismounting, its ethanol conversion is 99.0%, and selectivity of ethylene is 96.5%.
[embodiment 2]
3000 tons of/year producing ethylene from dehydration of ethanol devices are raw material with ethanol, adopt calandria type fixed bed reactor shown in Figure 1, adopt aluminium oxide catalyst.The shell side temperature is 430 ℃, and tube side is 410 ℃, is reflected under the normal pressure and carries out, and the raw material air speed is 0.8 hour
-1The reactor shell diameter is 1000 millimeters, the fused salt charge door is positioned at the axial of reactor upper body, 76 millimeters of heating tube external diameters, respectively in the axial insertion housing of reactor upper and lower housing, being concentric circles in cylindrical shell evenly distributes, the number of the convex shoulder in 40 millimeters of the big end external diameters of 45 millimeters of reaction tube external diameters, volute spring, the tube wall of reaction tube lower end is 2, and evenly distributes along the tube wall circumferencial direction.600 millimeters places along the circumferential direction evenly are provided with 4 radial temperature meters at the reactor interior diameter, highly locate to be provided with respectively 2 thermometers in the axial distance reactor lower end 1/3 and 2/3 of reactor.Record 4 radial temperatures and be respectively 408.5 ℃, 407.9 ℃, 408.0 ℃ and 409.5 ℃; Record 2 axial temperatures and be respectively 408.3 ℃ and 409.6 ℃.Equipment operates steadily, and ethanol conversion is 99.7%, and selectivity of ethylene is 97.1%.
[embodiment 3]
6000 tons of/year urea low pressure catalysis legal system melamine devices are raw material with urea, adopt calandria type fixed bed reactor shown in Figure 1, adopt the Alusil catalyst.The shell side temperature is 375 ℃, and tube side is 355 ℃, and reaction pressure is a normal pressure, and the raw material air speed is 0.6 hour
-1The reactor shell diameter is 1800 millimeters, and the fused salt charge door is positioned at the axial of reactor upper body, and heating tube is concentric circles and evenly distributes in the axial insertion housing on reactor top in cylindrical shell.Locate 300 millimeters of reactor interior diameters, 600 millimeters, 900 millimeters locate, 1000 millimeters places are provided with 4 radial temperature meters respectively, highly locate to be provided with respectively 3 thermometers in the axial distance reactor lower end 1/4,1/2,3/4 of reactor.Record 4 radial temperatures and be respectively 375.5 ℃, 376.6 ℃, 376.1 ℃ and 375.2 ℃; Record 3 axial temperatures and be respectively 374.9 ℃, 375.6 ℃ and 373.8 ℃.Equipment operates steadily, and conversion of raw material is 95.2%, and product yield is 93.0%.
[embodiment 4]
3000 tons/year 1,4-butanediol dehydration system oxolane device, with 1, the 4-butanediol is a raw material, adopts calandria type fixed bed reactor shown in Figure 1, employing Y zeolite catalyst.The shell side temperature is 300 ℃, and tube side is 285 ℃, and reaction pressure is a normal pressure, and the raw material air speed is 0.3 hour
-1The reactor shell diameter is 1000 millimeters, and the fused salt charge door is positioned at the axial of reactor upper body, and heating tube is concentric circles and evenly distributes in the axial insertion housing on reactor top in cylindrical shell.600 millimeters places along the circumferential direction evenly are provided with 3 radial temperature meters at the reactor interior diameter, highly locate to be provided with respectively 2 thermometers in the axial distance reactor lower end 1/3 and 2/3 of reactor.Record 3 radial temperatures and be respectively 285.8 ℃, 284.6 ℃ and 286.1 ℃; Record 2 axial temperatures and be respectively 283.9 ℃ and 284.6 ℃.Equipment operates steadily, and conversion of raw material is 99.8%, and the selectivity of oxolane is 96.5%.
[embodiment 5]
3000 tons of/year formamide dehydration hydrogen manufacturing fluoric acid devices are raw material with the formamide, adopt calandria type fixed bed reactor shown in Figure 1, adopt aluminium oxide catalyst.The shell side temperature is 320 ℃, and tube side is 300 ℃, and reaction pressure is a normal pressure, and the raw material air speed is 2.0 hours
-1The reactor shell diameter is 1200 millimeters, and the fused salt charge door is positioned at the axial of reactor upper body, and heating tube is concentric circles and evenly distributes in the axial insertion housing on reactor top in cylindrical shell.700 millimeters places along the circumferential direction evenly are provided with 3 radial temperature meters at the reactor interior diameter, highly locate to be provided with respectively 2 thermometers in the axial distance reactor lower end 1/3 and 2/3 of reactor.Record 3 radial temperatures and be respectively 298.8 ℃, 300.5 ℃ and 299.1 ℃; Record 2 axial temperatures and be respectively 298.9 ℃ and 300.6 ℃.Equipment operates steadily, and conversion of raw material is 96.0%, and product yield is 93.5%.
Claims (7)
1. method that is used for the endothermic reaction, reaction raw materials is contacted with catalyst in the calandria type fixed bed reactor reaction tube, reaction reaction of formation product, wherein raw material is selected from ethanol, butanediol, urea or formamide, described reactor comprises feed(raw material)inlet, reactor shell, goes up lower perforated plate, reaction tube, reacting product outlet, it is characterized in that being provided with in the reactor at least two heating tubes and stretches in the fused salt, is used to heat fused salt, fused salt is positioned at reactor shell, outside the reaction tube.
2. according to the described method that is used for the endothermic reaction of claim 1, it is characterized in that heating tube along the circumferential direction is evenly distributed.
3. according to the described method that is used for the endothermic reaction of claim 1, it is characterized in that heating tube is in the axial insertion housing of reactor upper body, or in the axial insertion housing of reactor lower part housing, or respectively in the axial insertion housing of reactor upper and lower housing.
4. according to the described method that is used for the endothermic reaction of claim 1, it is characterized in that in the tube wall of reaction tube lower end convex shoulder being set, volute spring is set on the convex shoulder.
5. according to the described method that is used for the endothermic reaction of claim 4, the number that it is characterized in that convex shoulder is 2～6, and evenly distributes along the tube wall circumferencial direction.
6. according to the described method that is used for the endothermic reaction of claim 4, it is characterized in that the big end external diameter of volute spring and the internal diameter of reaction tube are interference fit.
7. according to the described method that is used for the endothermic reaction of claim 6, the big end external diameter that it is characterized in that volute spring is greater than 1～6 millimeter of the internal diameter of reaction tube.
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| CN102784603A (en) * | 2012-07-12 | 2012-11-21 | 天津大学 | Gas distributor and vinyl acetate synthesis reactor comprising the same |
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| CN102160986B (en) * | 2011-03-15 | 2013-04-17 | 浙江大学 | Built-in spring tubular reactor |
| CN102872766B (en) * | 2012-10-21 | 2014-10-22 | 沈阳东方钛业股份有限公司 | Fluoridation reactor of fixed bed |
| CN105817186B (en) * | 2016-04-21 | 2018-10-19 | 广东椰氏实业股份有限公司 | A kind of entirety oil-bath type pipeline reactor and its implementation |
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