CN103071444B - Gas-liquid reaction device - Google Patents
Gas-liquid reaction device Download PDFInfo
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- CN103071444B CN103071444B CN201310035019.5A CN201310035019A CN103071444B CN 103071444 B CN103071444 B CN 103071444B CN 201310035019 A CN201310035019 A CN 201310035019A CN 103071444 B CN103071444 B CN 103071444B
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Abstract
The invention discloses a gas-liquid reaction device which comprises a reaction tank, wherein a gas-liquid mixing reactor is fixed inside the reaction tank; the reaction tank is communicated with the gas-liquid mixing reactor through a circulation pipe; a circulation pump is in series connection with a circulation pipeline; and the gas-liquid mixing reactor is a structure formed by connecting a gas chamber with a flow guide component through a gas-liquid mixing pipe. The device has the advantages that double circulation of gas-liquid materials can be realized; gas and liquid are fully mixed; the mass transfer efficiency of a chemical reaction is remarkably improved; raw materials are fully used; when a solid catalyst is needed, the liquid and the catalyst form a suspended solution with an agitator, so that the catalyst can circulate smoothly in the reaction device; the service life of the device is prolonged; and the maintenance cost of the device is lowered.
Description
Technical field
The present invention relates to gas-liquid technical field of chemical reactions, specifically relate to a kind of gas-liquid reaction apparatus.
Background technology
In chemical engineering industry, there is a large amount of gas liquid reactions, as the processing of industrial waste gas, catalytic hydrogenation, aminating reaction etc., existing in conventional gas-liquid reaction apparatus have absorption tower, Venturi tube, a jet ejectors etc., in absorption tower, liquid sprays from the top down from tower top, thereby gas is upwards realized gas-liquid mixed generation chemical reaction from bottom, jet ejectors is to utilize jet orifice to form negative pressure, gas is sucked, thereby realize gas-liquid mixed.But, several gas-liquid reaction apparatus all can not make that gas-liquid mixed is abundant, the long-acting rate of chemical time is low above, consumption of raw materials is large, so, technical staff once attempted developing multiple gas-liquid mixed and installed more fully, for example, (1) publication number is CN1745888, name is called the patent of " Liqiud-gas mixing device that utilizes jet circulation reaction characteristics ", the disclosed Liqiud-gas mixing device of this patent is to adopt liquid conduits interpolation gas inlet pipe, and gas-liquid is installed conic type diffuser in managing by induction and improved gas-liquid mixed effect.(2) publication number is CN201055774, and name is called the patent of " fluid jet gas-liquid mixture reaction unit ", and the disclosed Liqiud-gas mixing device of this patent is to adopt the mode that imports gas in guide shell lower end, makes gas-liquid mixed.But, even if done improved gas-liquid reaction apparatus, because gas-liquid mass transfer obstruction may cause, in pipeline, gas-liquid is parallel passes through, be difficult to realize abundant mixing, thereby reduce mass transfer mixing efficiency, and reaction unit can only be single realizes in gas recirculation access to plant, or realize liquid recirculation access to plant, reaction unit can not be realized intellectuality, inefficiency, operate complicated.
Prior art application gas liquid reaction still, while completing the reaction of the adjacent amino p-methyl benzenesulfonic acid of 2-nitro Catalyzed by p-Toluenesulfonic Acid Hydrogenation, temperature need to be more than 100 ℃, and pressure is more than 2.0 MPa, and the whole reaction time needs 3h just can complete.Apply gas-liquid reaction apparatus temperature of the present invention and only need 72-78 ℃, pressure only needs 25kPa, the time of whole reaction only needs 45 minutes, when hydrogen and 2-nitro p-methyl benzenesulfonic acid solution mixing generation chemical reaction, gas enters air chamber again through condenser, liquid flows back to retort, through circulating pump, be delivered to the air chamber of gas-liquid mixed reactor, hybrid reaction again, thereby at reacting tank body, realize two circulations of gas-liquid material outward, in gas-liquid mixed reactor, realizing three times fully mixes, improve the efficiency of chemical reaction, therefore the amino p-methyl benzenesulfonic acid yield of neighbour obtaining is high, material reaction is complete, save reaction raw materials, time-saving energy-saving, convenient to operation.
Summary of the invention
For solving the problems of the technologies described above, the invention discloses a kind of gas-liquid reaction apparatus, can realize two circulations of gas-liquid material, improve utilization of materials, make gas-liquid mixed abundant simultaneously, improve chemical reaction mass-transfer efficiency.
For achieving the above object, technical scheme of the present invention is, a kind of gas-liquid reaction apparatus, this device comprises retort, in the inner fixedly gas-liquid mixing reactor of retort, the structure that gas-liquid mixed reactor is connected and composed by gas-liquid mixed pipe by air chamber and guiding subassembly, retort is communicated with gas-liquid mixed reactor by circulation pipe, circulation pipe pipeline is in series with circulating pump, and preferred circulating pump is infinitely variable speeds type, and capable of regulating flow quantity size changes whole reaction mass cycle-index.Flow is large, and in the unit interval, often, gas-liquid mass transfer is abundant, reaction efficiency is high for gas-liquid cycle; Otherwise flow is little, gas-liquid mixed number of times is few, and material mass transfer, reaction efficiency are low.Above-mentioned guiding subassembly comprises mozzle A, mozzle B, flared tube, flared tube is fixed between gas-liquid mixed pipe and mozzle A, mozzle A is connected with mozzle B is nested, the caliber of gas-liquid mixed pipe is less than the caliber of mozzle A, the bottom of mozzle A and mozzle B has one or more pod apertures, and the diameter of pod apertures is less than 5mm.While utilizing gas-liquid reaction apparatus work of the present invention, liquid enters after retort, through circulating pump, be delivered to circulation pipe, circulation pipe is passed in the air chamber in gas-liquid mixed reactor, gas enters air chamber, during the nozzle ejection of the liquid now with certain pressure on circulation pipe, form high-velocity fluid, and mineralization pressure falls around nozzle, gas under negative pressure state is brought into gas-liquid mixed reactor mixing tube by high-speed liquid injection stream with spiral entrainmenting like this, each alternate material close contact of this one-phase, reactant is dispersed, suspend, form whole turbulent flow, thereby improving mass-transfer efficiency accelerated reaction carries out.Gas-liquid mixture out increases by flared tube static pressure from gas-liquid mixed pipe, and turbulence state changes formation secondary and mixes mass transfer again, reacts simultaneously.Mozzle A bottom has perforate, and gas-liquid mixture enters into mozzle B from these apertures, can again be subject to the shear action of pore, further strengthens gas-liquid mixed mass transport process, and guiding subassembly has guaranteed gas-liquid mixed efficiency for the third time.In addition, a plurality of apertures that mozzle A and mozzle B bottom have, guarantee that the pulverulent solids catalyst that chemical reaction needs can not stop up mozzle.Finally, the gas-liquid mixture that flow into mozzle B flows back in retort on its top, remaining liquid or catalyst flow back to retort by the pod apertures of mozzle B, now, the gas that does not complete chemical reaction is separated with liquid realization, and gas overflows liquid level in retort, by condenser, again flow into circular response in air chamber, liquid is delivered in air chamber circular response again in the bottom of retort through circulation pipe, has so also just realized the two circulations of gas-liquid material.
In gas-liquid reaction apparatus of the present invention, on described circulation pipe pipeline, be also connected with heat exchanger, thermal source can be provided, complete the chemical reaction that needs heating.
Described retort top sidewall connects condenser, the top of condenser has exhaust outlet, exhaust outlet is communicated with air chamber by being fixed with the pipeline of check valve, and unreacting gas can enter air chamber again and react with liquid-circulating, and nontoxic tail gas also can be discharged by the exhaust outlet on top.
Fixing angle-inserting type magnetically-actuated paddle also in the sidewall locations of retort bottom, can make it to form suspension to there being the liquid of solid powder th-1 catalyst to stir, so that loop passages such as the smooth and easy nozzle that passes through circulation pipe of material and pod apertures.
To sum up, gas-liquid reaction apparatus of the present invention can be realized the two Matter Transfers of gas-liquid, when gas-liquid mixture is flowed through respectively gas-liquid mixed section, flared tube, mozzle A, three strengthenings of gas-liquid material mix, significantly improved chemical reaction mass-transfer efficiency, raw material is fully utilized, and can guarantee, when needs solid catalyst, mixer can make liquid and catalyst form aaerosol solution, so that it is unobstructed to circulate in reaction unit, the service life of extension fixture, the maintenance cost of reduction device.
Accompanying drawing explanation
--Fig. 1 is gas-liquid reaction apparatus of the present invention;
Symbol description in figure, 1, charging aperture; 2, discharging opening; 3, retort; 4, gas-liquid mixed reactor; 41, air chamber; 42, gas-liquid mixed pipe; 43, guiding subassembly; 431, mozzle A; 432, mozzle B; 433, flared tube; 434, pod apertures; 5, circulation pipe; 6, circulating pump; 7, heat exchanger; 8, angle-inserting type magnetically-actuated paddle; 9, condenser; 10, check valve; 11, Pressure gauge; 12, condenser exhaust outlet.
The specific embodiment
Below in conjunction with specific embodiment, further illustrate summary of the invention.
As shown in Figure 1, gas-liquid reaction apparatus of the present invention, this device comprises retort 3, liquid and catalyst are all that the charging aperture 1 retort enters in retort, retort inside is fixed with gas-liquid mixed reactor 4, retort bottom opening connects circulation pipe 5, one side of circulation pipe is communicated with gas-liquid mixed reactor, opposite side is discharging opening 2, when reaction completes, can open the valve on discharging opening, facilitate the discharge of material, on this circulation pipe pipeline, go back fixed cycles pump 6, circulating pump can be delivered to the liquid material in retort gas-liquid mixed reactor, so there is Pressure gauge 11 on this pipeline, circulation pipe is exactly the general liquid line that carries nozzle in this area, it can be spurted into liquid in gas-liquid mixed reactor.
Inventive point of the present invention is the structure of described gas-liquid mixed reactor: top is that air chamber 41, bottom are guiding subassembly 43, and air chamber is communicated with guiding subassembly by gas-liquid mixed pipe 42.Above-mentioned circulation pipe is passed in gas-liquid mixed reactor, concrete is exactly to be passed in air chamber, and liquid sprays and enters gas-liquid mixed pipe, and gas indoor gas is entrainmented and taken away, gas-liquid mixture is mixed to form turbulence state in gas-liquid mixed pipe and flared tube, carries out mass transfer, reaction simultaneously.
Above-mentioned guiding subassembly comprises mozzle A431, mozzle B432, flared tube 433, and flared tube is fixed between gas-liquid mixed pipe and mozzle A, and mozzle A and the nested caliber that is connected gas-liquid mixed pipe of mozzle B are less than the caliber of mozzle A.Each structure in guiding subassembly all chooses the machine-shaping of suitable assembly one.
In the bottom of above-mentioned mozzle A and mozzle B, have one or more pod apertures 434, the diameter of pod apertures is less than 5mm.
Except above-mentioned feature, gas-liquid reaction apparatus of the present invention, on the circulation line of fixed cycles pump, is also fixed with heat exchanger 7; Fixing angle-inserting type magnetically-actuated paddle 8 in the sidewall locations of retort bottom; Retort top sidewall also connects condenser 9.
Above-mentioned condenser top has gas exhaust port 12, and exhaust outlet is communicated with air chamber by having the passage of check valve 10.
List several examples of utilizing apparatus of the present invention to complete chemical reaction below.
Utilize the present invention's gas-liquid reaction apparatus as shown in Figure 1, complete the reaction of the adjacent amino p-methyl benzenesulfonic acid of 2-nitro Catalyzed by p-Toluenesulfonic Acid Hydrogenation, concrete operations are as follows: (1) adds 2-nitro p-methyl benzenesulfonic acid 430g in the 3L beaker that 1500ml distilled water is housed, heating for dissolving forms solution, while hot solution is transferred in retort by charging aperture, add fineness is 80-120 object Raney nickel 23g simultaneously, starts magnetically-actuated paddle 8 and stirs 1-2 minute, (2) start circulating pump and open heat exchanger, the temperature of heat exchanger, between 72-78 ° of C, then is opened condenser, and hydrogen is passed into air chamber, passes into after 1-2 minute, closes the exhaust outlet of condenser, the check valve of outwarding winding between condenser and air chamber, (3) first two steps are all transferred to proper states by the assembly of device, 2-nitro p-methyl benzenesulfonic acid solution starts to mix generation chemical reaction with hydrogen, in air chamber, the liquid that is evacuated to circulation pipe through circulating pump ejects with hydrogen and starts to mix, first gas-liquid mixed pipe in gas-liquid mixed reactor, flow into again in guiding subassembly, gas-liquid mixed pipe is less than the caliber of the mozzle A in guiding subassembly, gas-liquid mixture is that the spiral state of negative pressure is inhaled in mozzle A, is now high efficiency gas-liquid mixed for the first time, before being inhaled into mozzle A, gas-liquid mixture also can pass through flared tube, pressure is strengthened and form gas-liquid turbulence state, for high efficiency gas-liquid mixed for the second time, during mixing, there is chemical reaction, when last gas-liquid mixture is flowed through in mozzle A, pod apertures through mozzle A bottom flows out, gas-liquid mixture is in so narrow and small passage, it is now abundant gas-liquid mixture mixture for the third time, significantly improve chemical reaction efficiency, the gas of complete reaction and liquid is not after the mozzle B that flows through, gas is on the top of retort, in condenser is passed into air chamber, recycling, liquid flows in the circulation pipe of retort bottom, be transported to again in gas-liquid mixed reactor and recycle, (4) utilize gas-liquid reaction apparatus of the present invention to produce adjacent amino p-methyl benzenesulfonic acid, whole reaction temperature is between 72-78 ℃, in retort, gas pressure intensity is 25kPa, at 2-nitro p-methyl benzenesulfonic acid and hydrogen reaction, after 35 minutes, stop passing into hydrogen, continue reaction after 10 minutes, after sampling detects definite reaction, close circulating pump and heat exchanger, the amino p-methyl benzenesulfonic acid of neighbour obtaining is got rid of from discharging opening, the valve closing of this passage during reaction, after reaction, valve can be outwarded winding to discharge reactant, the reacting rear material of discharging is carried out to separation and purification, the amino p-methyl benzenesulfonic acid purity of neighbour obtaining reaches more than 98%, unreacted 2-nitro p-methyl benzenesulfonic acid is lower than 0.2%.
Embodiment bis-: utilize gas-liquid reaction apparatus of the present invention synthetic 2,3-diacetyl-oxime, butanone and nitrous ether (ethyl nitrite) generation chemical reaction make 2,3-diacetyl-oxime, this chemical reaction occurs under condition of normal pressure, due to a large amount of heat releases of reaction, can bring harmful gas nitrous ether (ethyl nitrite) to overflow system, often with tail gas form, discharge to environment and bring harm, adopt the inventive method to adopt the two circulations of gas-liquid can make butanone fully react with nitrous ether (ethyl nitrite), significantly reduce nitrous ether (ethyl nitrite) and overflow system.Concrete operation step is as follows:
(1) butanone solution enters retort by charging aperture, heat exchange temperature is set in to 48-55 ℃, start condenser, close the exhaust outlet of condenser, the check valve of outwarding winding between condenser and air chamber, nitrous ether (ethyl nitrite) gas is passed into air chamber, start circulating pump, butanone liquid is through circulating pump, at heat exchanger, complete after heating, by circulation pipe, spurt into air chamber, with the nitrous ether (ethyl nitrite) gas mixed flow in air chamber through gas-liquid mixed pipe, via flared tube, enter again mozzle A, gas-liquid mixture finally flows into mozzle B by the aperture of mozzle A bottom, from mozzle B gas and fluid separation applications out, liquid flows back to retort and through circulating pump, circulates, gas enters air chamber through condenser, also recirculation, (2) nitrous ether (ethyl nitrite) gas reacts after 15 minutes in gas-liquid mixed mechanism with butanone liquid, stop passing into nitrous ether (ethyl nitrite) gas, continue reaction 10 minutes, close circulating pump and heat exchanger, by make 2,3-diacetyl-oxime is discharged from discharging opening, after separation and purification, obtain 2, the about 380g of 3-diacetyl-oxime, nitrous ether (ethyl nitrite) GAS ABSORPTION rate reaches more than 99.6%, after having reacted, gas can be discharged from the exhaust outlet of condenser, record nitrous ether (ethyl nitrite) emptying concentration 0.01-0.03%, reach the discharge standard of Ministry of environment's regulation.
Embodiment tri-: reaction unit of the present invention is used for the specific embodiment of aminating reaction: the main technique route that China's tertiary amine is produced is fatty alcohol catalyzing amination method, and the alcohol Amination Technique of most manufacturers is the forms that adopt stirred tank.Stirred-tank reactor is simple in structure, easily manufactured, but its mass transfer problem can not get good solution, and adopts the two recirculation reactor forms of gas-liquid can strengthen the mass transport process between gas-liquid-solid three-phase, addresses the above problem.
Adopt apparatus of the present invention, take higher aliphatic and dimethylamine gas is raw material, employing be take copper as the main ternary catalyst that appraises at the current rate, produce senior fat tertiary amine, production procedure, with embodiment bis-, finally show that the product quality mark of the senior fat tertiary amine of product is greater than 98 %, illustrates under identical inventory, apply reaction unit of the present invention, the aminating reaction time is than having shortened more than 50% with existing stirred tank reaction.In addition, its catalyst activity and selectively higher, consumption of raw materials is relatively less, and product yield is high, has obvious economic benefit.
Embodiment tetra-: the application of apparatus of the present invention in oxidation reaction, if paracresol is waste vanillic aldehyde product, its key intermediate is parahydroxyben-zaldehyde.It is the gas-liquid two-phase course of reaction that typically has solid catalyst to participate in that Catalytic Oxidation of Paracresol is produced parahydroxyben-zaldehyde, because reaction oxygen used solubility in methyl alcohol or ethanol equal solvent is less, the size of the paracresol reaction rate in oxygen and solvent is directly subject to the control of gas-liquid mixing efficiency.Adopt gas-liquid reaction apparatus of the present invention, can make paracresol and oxygen at gas-liquid mixed pipe, in flared tube and mozzle A, fully mix, reaction, greatly improved the conversion efficiency of gas-liquid mixed mass-transfer efficiency and paracresol, concrete grammar is: in retort, add methyl alcohol 1800mL and paracresol 216g+100g potassium hydroxide, stir while adding and add appropriate solid powdery catalyst to make mixed liquor simultaneously, by 58 ℃-75 ℃ of heat exchanger design temperatures, condenser access condensed water is also closed exhaust outlet, check valve on condenser and air chamber path, start again circulating pump, by circulation pipe, import paracresol reactant liquor and oxygen gas is accessed to air chamber, in gas-liquid mixed reactor, under alkali condition, Catalytic Oxidation of Paracresol becomes parahydroxyben-zaldehyde, fully the oxygen gas of reaction is not passed through condenser, check valve enters successive reaction in mixing reactor, paracresol reactant liquor enters in retort through retort bottom by circulation pipe again, after circulation 60min, react complete, stop passing into oxygen, continue reaction 5min, close down circulating pump and heat exchanger heater.Material is discharged from discharging opening, through separation and purification, can obtain the about 210g of parahydroxyben-zaldehyde.Use apparatus of the present invention oxidation time to shorten 90min, than existing reaction unit time shorten approximately 60%, parahydroxyben-zaldehyde yield reaches 86%, than adopting conventional stirred tank reaction, product yield improves more than 10%.
Gas-liquid reaction apparatus of the present invention can improve efficiency, the Reaction time shorten of polytype gas liquid reaction; the embodiment listing is only for further illustrating structure of the present invention; and the beneficial effect that brings of structure of the present invention; any restriction of not invention being made, all within the present invention's simple modification that content is made in fact and improvement all still belong to the protection domain of technical solution of the present invention.
Claims (5)
1. a gas-liquid reaction apparatus, this device comprises retort (3), at the inner fixedly gas-liquid mixing reactor (4) of retort, retort is communicated with gas-liquid mixed reactor by circulation pipe (5), on circulation pipe pipeline, be serially connected with circulating pump (6), it is characterized in that, retort top sidewall also connects condenser (9), described gas-liquid mixed reactor is the structure being connected and composed by gas-liquid mixed pipe (42) by air chamber (41) and guiding subassembly (43), guiding subassembly comprises mozzle A(431), mozzle B(432), flared tube (433), flared tube is fixed between gas-liquid mixed pipe and mozzle A, the nested inner side that is connected to mozzle B of mozzle A, the caliber that flared tube connects mozzle A end is greater than the caliber that connects gas-liquid mixed pipe end, mozzle A and mozzle B bottom have one or more pod apertures (434), the diameter of pod apertures is less than 5mm.
2. gas-liquid reaction apparatus according to claim 1, is characterized in that, the caliber of gas-liquid mixed pipe is less than the caliber of mozzle A.
3. gas-liquid reaction apparatus according to claim 1, is characterized in that, on the circulation line of described fixed cycles pump, is also serially connected with heat exchanger (7).
4. gas-liquid reaction apparatus according to claim 1, is characterized in that, fixing angle-inserting type magnetically-actuated paddle (8) also in the sidewall locations of described retort bottom.
5. gas-liquid reaction apparatus according to claim 1, is characterized in that, the top of described condenser has gas exhaust port (12), and exhaust outlet is communicated with air chamber by having the passage of check valve (10).
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| CN201310035019.5A CN103071444B (en) | 2013-01-30 | 2013-01-30 | Gas-liquid reaction device |
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| CN201310035019.5A CN103071444B (en) | 2013-01-30 | 2013-01-30 | Gas-liquid reaction device |
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| CN103071444B true CN103071444B (en) | 2014-12-10 |
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