CN103071444A - Gas-liquid reaction device - Google Patents
Gas-liquid reaction device Download PDFInfo
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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 the 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, such as the processing of industrial waste gas, catalytic hydrogenation, aminating reaction etc., existing in the gas-liquid reaction apparatus commonly used have absorption tower, Venturi tube, a jet ejectors etc., liquid sprays from the top down from the tower top in the absorption tower, thereby gas is upwards realized gas-liquid mixed generation chemical reaction from the bottom, jet ejectors is to utilize jet orifice to form negative pressure, gas is sucked, thereby realize gas-liquid mixed.But, above several gas-liquid reaction apparatus can not make all that gas-liquid mixed is abundant, the long-acting rate of chemical time is low, consumption of raw materials is large, so, the 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 the installation conic type diffuser improves the gas-liquid mixed effect to gas-liquid in the pipe by inducing.(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 the guide shell lower end, makes gas-liquid mixed.But, even if done improved gas-liquid reaction apparatus, gas-liquid is parallel in pipeline passes through because the gas-liquid mass transfer obstruction may cause, be difficult to realize abundant mixing, thereby reduce the mass transfer mixing efficiency, and in the realization gas recirculation access to plant that reaction unit can only be single, or realize liquid recirculation access to plant, reaction unit can not be realized intellectuality, inefficiency, the operation complicated.
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 simultaneously gas-liquid mixed abundant, improve the 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 the gas-liquid mixed reactor is connected and composed by the gas-liquid mixed pipe by air chamber and guiding subassembly, retort is communicated with the gas-liquid mixed reactor by circulation pipe, the circulation pipe pipeline is in series with circulating pump, and preferred circulating pump is the infinitely variable speeds type, and the capable of regulating flow quantity size changes whole reaction mass cycle-index.Flow is large, in the unit interval gas-liquid cycle often, gas-liquid mass transfer is abundant, reaction efficiency is high; Otherwise flow is little, and the 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 the 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.When utilizing gas-liquid reaction apparatus work of the present invention, after liquid enters retort, be delivered to circulation pipe through circulating pump, circulation pipe is passed in the air chamber in the gas-liquid mixed reactor, gas enters air chamber, during the nozzle ejection of the liquid that have certain pressure this moment 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 the high-speed liquid injection stream with spiral entrainmenting like this, each alternate material close contact of this one-phase, the reactant Uniform Dispersion, suspend, form whole turbulent flow, carry out thereby improve the mass-transfer efficiency accelerated reaction.Gas-liquid mixture out increases by the flared tube static pressure from the gas-liquid mixed pipe, and turbulence state changes the 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 the gas-liquid mixed mass transport process, and guiding subassembly has guaranteed gas-liquid mixed efficient 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.At last, the gas-liquid mixture that flow into mozzle B flows back in the retort on its top, remaining liquid or catalyst flow back to retort by the pod apertures of mozzle B, at this moment, do not finish the gas of chemical reaction and realize separating with liquid, gas overflows liquid level in retort, again flow into circular response in the air chamber by condenser, liquid then is delivered in the air chamber again circular response in the bottom of retort through circulation pipe, has so also just realized the two circulations of gas-liquid material.
In the gas-liquid reaction apparatus of the present invention, on the described circulation pipe pipeline, also be connected with heat exchanger, thermal source can be provided, finish 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 the pipeline that is fixed with check valve, and unreacting gas can enter air chamber and liquid-circulating reaction again, and nontoxic tail gas also can be discharged by the exhaust outlet on top.
Fixing angle-inserting type magnetically-actuated paddle also on the sidewall locations of retort bottom can stir the liquid that solid powder th-1 catalyst is arranged and make it to form suspension, so that smooth and easy nozzle and the loop passage such as pod apertures by circulation pipe of material.
To sum up, gas-liquid reaction apparatus of the present invention can be realized the two Matter Transfers of gas-liquid, the gas-liquid material was strengthened mixing three times when gas-liquid mixture was flowed through respectively gas-liquid mixed section, flared tube, mozzle A, significantly improved the chemical reaction mass-transfer efficiency, raw material is fully utilized, and can guarantee, when the needs solid catalyst, mixer can make liquid and catalyst form aaerosol solution, so that circulation is unobstructed in reaction unit, the service life of extension fixture, the maintenance cost of reduction device.
Description of drawings
--Fig. 1 is gas-liquid reaction apparatus of the present invention;
Symbol description among the 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
Further specify summary of the invention below in conjunction with specific embodiment.
As shown in Figure 1, gas-liquid reaction apparatus of the present invention, this device comprises retort 3, liquid and catalyst all are that the charging aperture 1 on the retort enters in the retort, retort inside is fixed with gas-liquid mixed reactor 4, the retort bottom opening connects circulation pipe 5, one side of circulation pipe is communicated with the gas-liquid mixed reactor, opposite side is discharging opening 2, when reaction is finished, can open the valve on the discharging opening, make things convenient for the discharge of material, go back fixed cycles pump 6 on this circulation pipe pipeline, circulating pump can be delivered to the liquid material in the retort gas-liquid mixed reactor, so Pressure gauge 11 is arranged on this pipeline, circulation pipe is exactly the general liquid line that carries nozzle in this area, and it can be spurted into liquid in the 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 the gas-liquid mixed reactor, concrete is exactly to be passed in the air chamber, and liquid sprays and enters the gas-liquid mixed pipe, gas in the air chamber is entrainmented take away, gas-liquid mixture mix to form turbulence state in gas-liquid mixed pipe and flared tube, carries out simultaneously mass transfer, reaction.
Above-mentioned guiding subassembly comprises mozzle A431, mozzle B432, flared tube 433, and flared tube is fixed between gas-liquid mixed pipe and the mozzle A, and mozzle A and the nested caliber of gas-liquid mixed pipe that is connected of mozzle B are less than the caliber of mozzle A.Each structure in the guiding subassembly all chooses the machine-shaping of suitable assembly one.
Have one or more pod apertures 434 in the bottom of above-mentioned mozzle A and mozzle B, 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, also is fixed with heat exchanger 7; Fixing angle-inserting type magnetically-actuated paddle 8 on 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 the passage with check valve 10.
The below lists several examples of utilizing apparatus of the present invention to finish chemical reaction.
Utilize the present invention's gas-liquid reaction apparatus as shown in Figure 1, finish the reaction of the adjacent amino p-methyl benzenesulfonic acid of 2-nitro Catalyzed by p-Toluenesulfonic Acid Hydrogenation, concrete operations are as follows: be equipped with 2-nitro p-methyl benzenesulfonic acid 430g adding in the 3L beaker of 1500ml distilled water (1), heating for dissolving forms solution, while hot solution is transferred in the retort by charging aperture, adding simultaneously fineness is 80-120 purpose Raney nickel 23g, starts magnetically-actuated paddle 8 and stirs 1-2 minute; (2) start circulating pump and open heat exchanger, the temperature of heat exchanger is opened condenser again between 72-78 ° of C, hydrogen is passed into air chamber, pass into 1-2 minute after, close the exhaust outlet of condenser, the check valve between condenser and the air chamber outwarded winding; (3) first two steps all are transferred to proper states with the assembly of device, 2-nitro p-methyl benzenesulfonic acid solution and hydrogen begin the mixed occurrence chemical reaction, in air chamber, the liquid that is evacuated to circulation pipe through circulating pump ejects with hydrogen and begins to mix, the gas-liquid mixed pipe of elder generation in the gas-liquid mixed reactor, flow into again in the guiding subassembly, the gas-liquid mixed pipe is less than the caliber of the mozzle A in the guiding subassembly, gas-liquid mixture is that the spiral state of negative pressure is inhaled among the mozzle A, and be the high efficiency gas-liquid mixed first time this moment; Be inhaled into before the mozzle A, gas-liquid mixture also can pass through flared tube, pressure is strengthened form the gas-liquid turbulence state, be the high efficiency gas-liquid mixed second time, chemical reaction occurs during mixing, when last gas-liquid mixture is flowed through among the mozzle A, pod apertures through mozzle A bottom flows out, gas-liquid mixture is in so narrow and small passage, be abundant gas-liquid mixture mixture for the third time this moment, significantly improve chemical reaction efficiency, the gas of complete reaction and liquid is not behind the mozzle B that flows through, and gas is on the top of retort, in condenser is passed into air chamber, recycling, liquid then flow in the circulation pipe of retort bottom, are transported in the gas-liquid mixed reactor recycling again; (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 ℃, gas pressure intensity is 25kPa in the retort, stop to pass into hydrogen after 35 minutes at 2-nitro p-methyl benzenesulfonic acid and hydrogen reaction, continue reaction after 10 minutes, after the sampling detection determines that reaction is finished, close circulating pump and heat exchanger, the adjacent amino p-methyl benzenesulfonic acid that obtains is got rid of from discharging opening, the valve closing of this passage during reaction, valve can be outwarded winding in order to discharge reactant after the reaction, the reacting rear material of discharging is carried out separation and purification, the adjacent amino p-methyl benzenesulfonic acid purity that obtains reaches more than 98%, and unreacted 2-nitro p-methyl benzenesulfonic acid is lower than 0.2%.
Prior art is used the gas liquid reaction still, and when finishing 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 finish.Use gas-liquid reaction apparatus temperature of the present invention and only need 72-78 ℃, pressure only needs 25kPa, the time of whole reaction only needed get final product in 45 minutes, when hydrogen and 2-nitro p-methyl benzenesulfonic acid solution mixed occurrence chemical reaction, gas enters air chamber again through condenser, liquid flows back to retort, be delivered to the air chamber of gas-liquid mixed reactor through circulating pump, hybrid reaction again, thereby outside reacting tank body, realize two circulations of gas-liquid material, in the gas-liquid mixed reactor, realize three times and fully mix, improve the efficient of chemical reaction, therefore the adjacent amino p-methyl benzenesulfonic acid yield that obtains is high, and material reaction is complete, save reaction raw materials, time-saving energy-saving, convenient to operation.
Embodiment two: 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 the condition of normal pressure, because a large amount of heat releases of reaction, can bring the harmful gas nitrous ether (ethyl nitrite) to overflow system, often discharge to environment with the tail gas form and bring harm, adopt the inventive method to adopt the two circulations of gas-liquid that butanone and nitrous ether (ethyl nitrite) are fully reacted, 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 48-55 ℃, start condenser, close the exhaust outlet of condenser, outward winding check valve between condenser and the air chamber, nitrous ether (ethyl nitrite) gas is passed into air chamber, start circulating pump, butanone liquid is through circulating pump, after heat exchanger is finished heating, spurt into air chamber by circulation pipe, with nitrous ether (ethyl nitrite) gas mixed flow in the air chamber through the gas-liquid mixed pipe, enter again mozzle A via flared tube, gas-liquid mixture flows into mozzle B by the aperture of mozzle A bottom at last, and from mozzle B gas and fluid separation applications out, liquid flows back to retort and circulates through circulating pump, gas enters air chamber through condenser, also recirculation; (2) nitrous ether (ethyl nitrite) gas and butanone liquid are after gas-liquid mixed mechanism reacts 15 minutes, stop to pass into nitrous ether (ethyl nitrite) gas, continue reaction 10 minutes, close circulating pump and heat exchanger, with make 2,3-diacetyl-oxime is discharged from discharging opening, after the separation and purification, obtain 2,3-diacetyl-oxime is 380g approximately, and nitrous ether (ethyl nitrite) GAS ABSORPTION rate reaches more than 99.6%, gas can be discharged from the exhaust outlet of condenser after reaction is finished, record nitrous ether (ethyl nitrite) emptying concentration 0.01-0.03%, reach the discharge standard of Ministry of environment's regulation.
Embodiment three: reaction unit of the present invention is used for the specific embodiment of aminating reaction: the main technique route of China's tertiary amine production is fatty alcohol catalyzing amination method, and the pure Amination Technique of most manufacturers is the forms that adopt stirred tank.Stirred-tank reactor is simple in structure, and is easily manufactured, but its mass transfer problem can not get good solution, and the two recirculation reactor forms of employing gas-liquid can be strengthened the mass transport process between the gas-liquid-solid three-phase, address the above problem.
Adopt apparatus of the present invention, take higher aliphatic and dimethylamine gas as raw material, the employing catalyst that appraises at the current rate take copper as main ternary, produce senior fat tertiary amine, production procedure draws the product quality mark of the senior fat tertiary amine of product greater than 98 % at last with embodiment two, illustrates under identical inventory, use 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 four: the application of apparatus of the present invention in oxidation reaction is waste vanillic aldehyde product such as paracresol, and 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 the used oxygen of reaction solubility in methyl alcohol or ethanol equal solvent is less, the size of the paracresol reaction rate in oxygen and the solvent directly is subjected to the control of gas-liquid mixing efficiency.Adopt gas-liquid reaction apparatus of the present invention, can make paracresol and oxygen at the gas-liquid mixed pipe, fully mix among flared tube and the mozzle A, reaction, greatly improved the conversion efficiency of gas-liquid mixed mass-transfer efficiency and paracresol, concrete grammar is: add methyl alcohol 1800mL and paracresol 216g+100g potassium hydroxide in retort, stir while adding and add simultaneously an amount of solid powdery catalyst and make mixed liquor, with 58 ℃-75 ℃ of heat exchanger design temperatures, condenser access condensed water is also closed exhaust outlet, check valve on condenser and the air chamber path, start again circulating pump, import the paracresol reactant liquor and oxygen gas is accessed air chamber by circulation pipe, in the gas-liquid mixed reactor under alkali condition Catalytic Oxidation of Paracresol become parahydroxyben-zaldehyde, fully the oxygen gas of reaction is not passed through condenser, check valve enters successive reaction in the mixing reactor, the paracresol reactant liquor enters in the retort through the retort bottom by circulation pipe again, circulation 60min afterreaction is complete, stop to pass into oxygen, continue reaction 5min, close down circulating pump and heat exchanger heater.Material is discharged from discharging opening, can obtain approximately 210g of parahydroxyben-zaldehyde through separation and purification.Use apparatus of the present invention oxidation time to shorten 90min, than existing reaction unit time shorten approximately 60%, the parahydroxyben-zaldehyde yield reaches 86%, than adopting conventional stirred tank to react, product yield improves more than 10%.
Gas-liquid reaction apparatus of the present invention can improve efficient, the Reaction time shorten of polytype gas liquid reaction; the embodiment that lists is only for further specifying structure of the present invention; and the beneficial effect that brings of structure of the present invention; be not any restriction that invention is made, all the present invention in fact the simple modification made of content and improving all still belong within the protection domain of technical solution of the present invention.
Claims (8)
1. gas-liquid reaction apparatus, this device comprises retort (3), at the inner fixedly gas-liquid mixing reactor (4) of retort, retort is communicated with the gas-liquid mixed reactor by circulation pipe (5), be serially connected with circulating pump (6) on the circulation pipe pipeline, it is characterized in that, described gas-liquid mixed reactor is the structure that is connected and composed by gas-liquid mixed pipe (42) by air chamber (41) and guiding subassembly (43).
2. gas-liquid reaction apparatus according to claim 1, it is characterized in that, described guiding subassembly comprises mozzle A(431), mozzle B(432), flared tube (433), flared tube is fixed between gas-liquid mixed pipe and the mozzle A, mozzle A is connected with mozzle B is nested.
3. gas-liquid reaction apparatus according to claim 2 is characterized in that, the caliber of described gas-liquid mixed pipe is less than the caliber of mozzle A.
4. gas-liquid reaction apparatus according to claim 2 is characterized in that, the bottom of described mozzle A and mozzle B has one or more pod apertures (434), and the diameter of pod apertures is less than 5mm.
5. gas-liquid reaction apparatus according to claim 1 is characterized in that, on the circulation line of described fixed cycles pump, also is serially connected with heat exchanger (7).
6. gas-liquid reaction apparatus according to claim 1 is characterized in that, fixing angle-inserting type magnetically-actuated paddle (8) also on the sidewall locations of described retort bottom.
7. gas-liquid reaction apparatus according to claim 1 is characterized in that, described retort top sidewall also connects condenser (9).
8. gas-liquid reaction apparatus according to claim 7 is characterized in that, the top of described condenser has gas exhaust port (12), and exhaust outlet is communicated with air chamber by the passage with check valve (10).
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| CN103537248A (en) * | 2013-10-30 | 2014-01-29 | 江苏泰丰化工有限公司 | Mixed alkali recovery venturi injection type reaction device |
| CN103657574A (en) * | 2013-11-27 | 2014-03-26 | 杭州海虹精细化工有限公司 | Device for preparing ADC (azodicarbonamide) foaming agent by self-suction oxidation |
| CN104056587A (en) * | 2014-06-20 | 2014-09-24 | 王玙璠 | Energy-saving reaction kettle |
| CN104177862A (en) * | 2013-11-06 | 2014-12-03 | 江苏泰丰化工有限公司 | Sodium-potassium ratio adjusting device of device for recovering mixed alkali from indigo products |
| CN105642220A (en) * | 2016-01-06 | 2016-06-08 | 南京大学 | Multi-stair circulating type jet reactor |
| CN105749849A (en) * | 2016-04-26 | 2016-07-13 | 江苏安邦电化有限公司 | Venturi circulation loop reactor for continuous production of ethephon and method |
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| CN112237896A (en) * | 2020-09-21 | 2021-01-19 | 中国石油大学(华东) | Novel mixing-enhanced reactor for alkylation of ionic liquid |
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| CN114085169A (en) * | 2021-11-06 | 2022-02-25 | 普林斯(安庆)医药科技有限公司 | Preparation and processing technology of organic amide |
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| CN103537248A (en) * | 2013-10-30 | 2014-01-29 | 江苏泰丰化工有限公司 | Mixed alkali recovery venturi injection type reaction device |
| CN104177862A (en) * | 2013-11-06 | 2014-12-03 | 江苏泰丰化工有限公司 | Sodium-potassium ratio adjusting device of device for recovering mixed alkali from indigo products |
| CN103657574A (en) * | 2013-11-27 | 2014-03-26 | 杭州海虹精细化工有限公司 | Device for preparing ADC (azodicarbonamide) foaming agent by self-suction oxidation |
| CN104056587A (en) * | 2014-06-20 | 2014-09-24 | 王玙璠 | Energy-saving reaction kettle |
| CN105642220A (en) * | 2016-01-06 | 2016-06-08 | 南京大学 | Multi-stair circulating type jet reactor |
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| CN111302360A (en) * | 2020-04-20 | 2020-06-19 | 扬州天启新材料股份有限公司 | Cyanogen chloride preparation process for cyanate resin synthesis |
| CN111302360B (en) * | 2020-04-20 | 2021-09-21 | 扬州天启新材料股份有限公司 | Cyanogen chloride preparation process for cyanate resin synthesis |
| CN112237896A (en) * | 2020-09-21 | 2021-01-19 | 中国石油大学(华东) | Novel mixing-enhanced reactor for alkylation of ionic liquid |
| CN114315518A (en) * | 2020-09-29 | 2022-04-12 | 北京诺维新材科技有限公司 | Chlorohydrination reaction device and application thereof |
| CN112535988A (en) * | 2020-11-18 | 2021-03-23 | 中广核环保产业有限公司 | Micro-nano bubble preparation device and preparation method thereof |
| CN112619588A (en) * | 2020-12-02 | 2021-04-09 | 辽宁圣德华星化工有限公司 | Tertiary amine production device and production method thereof |
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