CN101590385A - A kind of efficient ultrasonic recirculating-type reaction device - Google Patents
A kind of efficient ultrasonic recirculating-type reaction device Download PDFInfo
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- CN101590385A CN101590385A CNA2008101736356A CN200810173635A CN101590385A CN 101590385 A CN101590385 A CN 101590385A CN A2008101736356 A CNA2008101736356 A CN A2008101736356A CN 200810173635 A CN200810173635 A CN 200810173635A CN 101590385 A CN101590385 A CN 101590385A
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- supersonic generator
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Abstract
The present invention is improved circulating reactor equipment, mainly comprises parts such as tower body, heat exchanger, gas distributor, supersonic generator.Can improve the service efficiency of tower greatly by the introducing of supersonic generator, this reactor catalysis, oxidation, hydrogenation, hydrogen cyanide/ammonia remove and precipitation, crystallization etc. exist in the heterogeneous system of chemical field extensive use are arranged, this equipment has the reaction efficiency height, and enlarge-effect is little, mass-and heat-transfer good, low power consumption and other advantages.
Description
Technical field
The present invention relates to a kind of new-type gas-liquid-solid three-phase circulation reaction unit, specifically, relate to a kind of recirculating-type reaction device that is equipped with supersonic generator.
Background technology
The gas-liquid-solid three-phase system is a modal system in the chemical industry, and its effective mass-and heat-transfer is the maximum engineering problem of this system.Though devices such as fixed bed, fluid bed, continuous still reaction have obtained to use widely, particularly circulating reactor is that power is a kind of energy-efficient equipment by the difference in specific gravity that gas produced, though some application of this device, but it is not general, than the mass-and heat-transfer efficient height of fixed bed, fluid bed and bubble tower etc., be easy to amplify, power consumption lacks, being is worth a kind of novel reactor of using.But this reactor in use still exists further raising mass-transfer efficiency, improve distribution of gas, further strengthen three requirements such as practise physiognomy.
We discover that ultrasonic introducing can well can prevent that crystal is further long and better activate and upgrade catalyst surface with more miniaturization of bubble, improves the mass-and heat-transfer of boundary.This reactor is all to embody good effect at intermittent reaction or in continuous reaction, and the efficient mass transfer tower of this macroscopic view is a maximum bright spot of the present invention than the reactor of strengthening intermolecular decentralized photo combination on the microcosmic.
Summary of the invention
The effective assembled highly-effective reaction unit that the purpose of this invention is to provide a kind of supersonic generator and circulation flow reactor.It can be widely used in removing and technologies such as precipitation, crystallization of catalysis, oxidation, hydrogenation, hydrogen cyanide/ammonia.
Specifically, the invention provides a kind of ultrasonic recirculating-type reaction device, its basic structure is the circulating reactor of the built-in guide shell of tower, internal or external ultrasonic generator, gas distributor and outer circulation pipeline.It comprises parts such as tower body 1, diversing bucket 2, heat exchanger 3, gas distributor 4 and supersonic generator 5, and tower body is provided with discharging opening 6, air inlet 7, drain 8 and charging aperture 9.Wherein, heat exchanger 3 is preferably outer circulation type, and gas distributor 4 is positioned at tower, places the below of diversing bucket 2 in the tower.Ultrasound reactor 5 places outside Ta Nei and/or the tower.When placing in the tower, be preferably placed under the diversing bucket or the multistage diversing bucket between the gap, under the preferred diversing bucket.When placing tower outer, can place in the tower body outer circulation pipeline or pipeline is outer or place heat exchanger inside.
Circulating reactor of the present invention is, for example, and the reaction tower of circulation type or reactor or pressure vessel, for example, the tank reactor of circulation type, tubular reactor, airlift reactor, tower reactor.Among the present invention, circulating reactor is made of tower body 1, diversing bucket 2 and heat exchanger 3.Tower body 1 is equivalent to reaction tower or reactor or pressure vessel.
Specifically, the circulating reactor that the present invention equips supersonic generator is, for example, the tank reactor that has the built-in ultrasonic generator of liquid cycle specificity, the tubular reactor with liquid cycle specificity of external supersonic generator, the airlift reactor with liquid cycle specificity of external or built-in ultrasound reactor, airlift reactor with external supersonic generator of liquid cycle specificity, tower reactor with built-in supersonic generator of liquid cycle specificity, tower reactor etc. with external supersonic generator of liquid cycle specificity.More preferably, the airlift reactor of built-in supersonic generator, have the tower reactor of the built-in supersonic generator of liquid cycle specificity.
The outer circulation of reactor can be active cycle and passive circulation among the present invention, and preferred active cycle is promptly used the pump forced circulation.Active cycle helps external heat exchanger and carries out heat exchange, also helps the liquid circulation, has strengthened liquid mass transfer and heat transfer.
Apparatus of the present invention exist
Small testing device,
Pilot-plant and
Large-scale production plant successfully use.Use to confirm more than 1 year that apparatus of the present invention have fully that treating capacity is big, mass-and heat-transfer good, energy consumption is low and characteristics such as selectivity height.When being used for preparing glyphosate by oxidizing N-Phosphonomethyl iminodiacetic acid in air, carbon dioxide and preparing nano-calcium carbonate (being removing of the causticizing process washing, hydrogen cyanide or the ammonia that prepare calcium carbonate, material etc.), its dispersion effect is suitable with the high speed dispersion device.
Experiment showed, reactor of the present invention than high tens of times of the efficient of common still formula and tower reactor, even thousands of times.Apparatus of the present invention are successfully applied to, for example, 1) preparing glyphosate by oxidizing N-Phosphonomethyl iminodiacetic acid in air.Utilize ultrasonic wave and active carbon to be catalyst in apparatus of the present invention, oxygen-containing gas is an oxidant, preparing glyphosate by PMIDA catalytic oxidation, existing simple still reaction or fluid bed have been replaced, shortened the reaction time and increased mass transfer and heat transfer, and equipment investment is few, processing is simple.Use this device that conversion ratio in the preparing glyphosate by oxidizing N-Phosphonomethyl iminodiacetic acid in air technology is reached in a short period of time and be higher than common pressurization tank reactor and bubbling column reactor about 95% far away.2) causticizing process prepares the new technology of caustic soda and super fine calcium carbonate.Can produce micron-class superfine and nano-calcium carbonate easily in a large number with apparatus of the present invention, its particle diameter is about hundreds of nanometer to 1 micron, and particle size distribution range is narrow.3) contain hydrogen cyanide or ammonia wastewater recycling process.It is more energy-saving and cost-reducing than the method for chemical treatment and distillation that apparatus of the present invention can be simply and rapidly carried the hydrogen cyanide in the solution or ammonia by gas mode quickly falls to several ppm.
Description of drawings
Fig. 1 is a gas-liquid-solid three-phase recirculating-type reaction device of the present invention.
As shown in Figure 1, this device comprises the parts such as tower body 1, diversing bucket 2, heat exchanger 3, gas distributor 4 and supersonic generator 5, and tower body is provided with discharging opening 6, air inlet 7. Wherein, heat exchanger 3 is preferably outer circulation type, and gas distributor 4 is positioned at tower, places the below of diversing bucket 2 in the tower. Ultrasound reactor places outside Ta Nei and/or the tower. When placing in the tower, be preferably placed under the diversing bucket or the multistage diversing bucket between the gap, under the preferred diversing bucket. When placing tower outer, can place in the tower body outer circulation pipeline or pipeline is outer or place heat exchanger inner.
Most preferably, apparatus of the present invention adopt built-in supersonic generator, namely at tower body 1 interior installation supersonic generator. Supersonic generator can be installed in the below of gas distributor outlet in the tower. Require to select supersonic generator and the pull bar form of different capacity according to difference. Around supersonic generator, it is liquid material. Heat exchanger is heat-exchange apparatus, can carry out heating and cooling to material.
Supersonic generator is anyly can cause hyperacoustic equipment, and ultrasonic wave is delivered to the mechanical wave of reaction system by the solid-liquid medium, and its general frequency is greater than 15KHz. Equipment comprising the supersonic generator combination of using different frequency. Supersonic generator can be block or other shape, can be internal or external at the energy effective communication to any position of feed liquid system, but to place tower bottom or bottom as best.
For example, in built-in reactor, supersonic generator is in liquid material, the direction that its ultrasonic wave that sends and gas enter in the tower is consistent, the ultrasonic wave that acts on material produces vibration, produce the effect of vibration of linear alternation, simultaneously bubble is smashed dispersion, can mix gas-liquid-solid three-phase more even.
Gas distributor can adopt various porous/micropore distributor, to reach technical indicator and energy-saving and cost-reducing as prerequisite.
Embodiment
Following description is to specify of the present invention, should not regard limitation of the present invention as.
Embodiment 1:
Diameter 160mm, height is the tower body 1 of 2000mm, air inlet at the bottom of the tower, cat head has drain 8 and Pressure gauge, and there is thermometer at tower body 1 middle part, and tower body is established charging aperture 9 and discharging opening 6, built-in supersonic generator 5 at the bottom of the tower.
At diameter 160mm, height is interior 500 gram active fruit shell carbons, the 12000g water of adding of the stainless steel void tower of 2000mm, 3000 gram PMIDAs, 25% ammoniacal liquor, 900 grams, heating, oxygen is fed reaction solution, gas line speed 0.03m/s, control tower internal pressure 0.3MPa opens supersonic generator (200KHz, power is 50W), temperature rises to 67 ℃, and the phosphorus spectrum detects to the PMIDA complete reaction glyphosate reaction selectivity 89.6%.After reaction finishes, the filter activity charcoal, filtrate is adjusted pH=2 with 36% hydrochloric acid, obtains glyphosate 960g at last, content 95.33%.
Embodiment 2:
Diameter 50mm, height are the interior circulation airlift reactor 1 of 800mm, diversing bucket 2 height 300mm, and bottom inflow, Pressure gauge, thermometer and drain 8 are arranged at the top, the external supersonic generator 5 in tower bottom and crown center part side.
In tower, add 7.50 gram active carbons, 1000 gram water, 122 gram PMIDAs.Heating feeds reaction solution with air, gas line speed 0.10m/s, control tower top pressure 0.3MPa, open supersonic generator (80KHz, power are 80W), temperature rises to 75 ℃, the phosphorus spectrum detects to the PMIDA complete reaction, reacts glyphosate reaction selectivity 94.0% about 1.0 hours.
Embodiment 3:
Get waste water in example 2 reactors, feed the compressed air stripping and remove cyanogen, satisfactory for result, concrete data see the following form:
| Lot number | Treatment conditions | Before handling (ppm) | Handle back (ppm) |
| 1 | Get waste water in reactor ventilation treatment 1h | CN -：600 | CN -：20.0 |
| 2 | Get waste water 500g in reactor, logical 0.1m 3The air stream stripping of/h is handled 2h, continues stripping behind the sample analysis and handles 3.5h | CN -：600 | 2.0h sample CN -: 10.0 5.5h sample CN -：1.78 |
| 3 | Get waste water 530g in reactor, add 2g hydrochloric acid (37%), logical 0.1m 3The air stripping of/h is handled 1h, and behind the sample analysis, stripping 4h once more ventilates | CN -：600 | 1.0h sample CN -: 10.0 5.0h sample CN -：1.64 |
| 4 | Get waste water 525g in reactor, logical 0.2m 3The air stripping of/h is handled 1h | CN -：600 | CN -：15.0 |
Embodiment 4:
Because it is obvious that blow-off method removes the cyanogen effect, handle for the removal of ammonia, also can adopt and carry out the stripping processing under the high pH condition of being equipped in of example 3, experiment shows that blow-off method also can effectively remove the ammonia in the effluent brine.After stripping was handled, the ammonia more than 90% can be removed, and sees the following form:
Example 5
Diameter 400mm, height are the interior circulation airlift reactor 1 of 6000mm, diversing bucket 2 height 3500mm, and diameter is 300mm, bottom inflow, Pressure gauge, thermometer and drain 8 are arranged at the top, the built-in supersonic generator 5 in the bottom of bottom and air inlet 7.At 5% calcium chloride/ammonia spirit or calcium glycine solution bubbling air and carbon dioxide gas mixture, the particle diameter that can obtain calcite shape or sphere is the fine calcium carbonate of 200nm-1 μ m, and its every index and serviceability all are better than existing calcium carbonate.
The detailed description that the present invention did is enough detailed to those skilled in the art, and the method that can utilize this patent to provide.In addition, various replacements, that revise and the improved method that can obviously find out from top disclosed content does not break away from the spirit and scope of this patent.
Claims (7)
1, a kind of ultrasonic recirculating-type reaction device, it comprises tower body (1), diversing bucket (2), heat exchanger (3), gas distributor (4) and supersonic generator (5), tower body is provided with discharging opening (6), air inlet (7), wherein, heat exchanger (3) is an outer circulation type, and gas distributor (4) is positioned at tower, place the below of diversing bucket (2) in the tower, ultrasound reactor (5) places tower body (1) interior and/or outer.
2, according to the reaction unit of claim 1, wherein, supersonic generator (5) places in the tower body (1), under the diversing bucket or the gap between the multistage diversing bucket, under the preferred diversing bucket.
3, according to the reaction unit of claim 1, wherein, supersonic generator (5) places outside the tower body (1), can place in the tower body outer circulation pipeline or pipeline is outer or place heat exchanger inside, preferably places in the pipeline.
4, according to the reaction unit of claim 2, wherein, supersonic generator (5) is positioned at the bottom of the tower above to the position of diversing bucket (2) below the top.
5, according to the reaction unit of claim 1, diversing bucket can be n section, n 〉=1.
6, according to the reaction unit of claim 1, charging aperture and discharging opening do not limit particular location.
7, according to the reaction unit of claim 1, outer circulation can be active cycle and passive circulation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101736356A CN101590385A (en) | 2008-05-28 | 2008-11-03 | A kind of efficient ultrasonic recirculating-type reaction device |
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| CN200810113112 | 2008-05-28 | ||
| CN200810113112.2 | 2008-05-28 | ||
| CNA2008101736356A CN101590385A (en) | 2008-05-28 | 2008-11-03 | A kind of efficient ultrasonic recirculating-type reaction device |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102302919A (en) * | 2011-06-24 | 2012-01-04 | 华南理工大学 | Multi-frequency ultrasonic parallel radiation gas-liquid mass-transfer reaction device |
| CN102690411A (en) * | 2012-06-11 | 2012-09-26 | 北京旭阳化工技术研究院有限公司 | Method for copolymerizing carbon dioxide and propylene oxide with circulation flow reactor |
| CN102924957A (en) * | 2011-08-09 | 2013-02-13 | 江苏泰丰化工有限公司 | New tower type oxidation technology for indigo blue |
| CN104399272A (en) * | 2014-11-13 | 2015-03-11 | 中国科学院广州能源研究所 | Whole-process reaction type reaction rectification apparatus |
| CN106323706A (en) * | 2015-07-03 | 2017-01-11 | 中国石油化工股份有限公司 | Device for collecting oil component from liquid carbon dioxide containing oil component and extraction equipment using the same |
| CN107043150A (en) * | 2016-02-05 | 2017-08-15 | 江苏星晨环保集团有限公司 | A kind of ultrasonic Airlift circulating reactor |
| CN108745235A (en) * | 2018-08-24 | 2018-11-06 | 西南大学 | Circulation ultrasonic nano particle dispersion reactor in a kind of gas-lifting type |
| CN110099741A (en) * | 2016-11-02 | 2019-08-06 | 陶氏环球技术有限责任公司 | FCC reactor comprising air deflector |
| CN111007153A (en) * | 2018-10-08 | 2020-04-14 | 浙江大学 | Detection method for gas-liquid dispersion state of jet bubbling reactor |
| CN111036149A (en) * | 2019-12-02 | 2020-04-21 | 河南金鹏化工有限公司 | Water-washing continuous production process and device for thiodicarb |
-
2008
- 2008-11-03 CN CNA2008101736356A patent/CN101590385A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102302919A (en) * | 2011-06-24 | 2012-01-04 | 华南理工大学 | Multi-frequency ultrasonic parallel radiation gas-liquid mass-transfer reaction device |
| CN102302919B (en) * | 2011-06-24 | 2013-08-07 | 华南理工大学 | Multi-frequency ultrasonic parallel radiation gas-liquid mass-transfer reaction device |
| CN102924957A (en) * | 2011-08-09 | 2013-02-13 | 江苏泰丰化工有限公司 | New tower type oxidation technology for indigo blue |
| CN102924957B (en) * | 2011-08-09 | 2014-11-26 | 江苏泰丰化工有限公司 | New tower type oxidation technology for indigo blue |
| CN102690411A (en) * | 2012-06-11 | 2012-09-26 | 北京旭阳化工技术研究院有限公司 | Method for copolymerizing carbon dioxide and propylene oxide with circulation flow reactor |
| CN102690411B (en) * | 2012-06-11 | 2014-07-23 | 北京旭阳化工技术研究院有限公司 | Method for copolymerizing carbon dioxide and propylene oxide with circulation flow reactor |
| CN104399272A (en) * | 2014-11-13 | 2015-03-11 | 中国科学院广州能源研究所 | Whole-process reaction type reaction rectification apparatus |
| CN104399272B (en) * | 2014-11-13 | 2016-06-08 | 中国科学院广州能源研究所 | A kind of omnidistance reaction formula reactive distillation device |
| CN106323706A (en) * | 2015-07-03 | 2017-01-11 | 中国石油化工股份有限公司 | Device for collecting oil component from liquid carbon dioxide containing oil component and extraction equipment using the same |
| CN106323706B (en) * | 2015-07-03 | 2019-05-07 | 中国石油化工股份有限公司 | The device and extraction equipment of oil content are collected from the liquid carbon dioxide dissolved with oil content |
| CN107043150A (en) * | 2016-02-05 | 2017-08-15 | 江苏星晨环保集团有限公司 | A kind of ultrasonic Airlift circulating reactor |
| CN110099741A (en) * | 2016-11-02 | 2019-08-06 | 陶氏环球技术有限责任公司 | FCC reactor comprising air deflector |
| CN110099741B (en) * | 2016-11-02 | 2022-03-01 | 陶氏环球技术有限责任公司 | Fluidized catalytic reactor comprising flow directors |
| CN108745235A (en) * | 2018-08-24 | 2018-11-06 | 西南大学 | Circulation ultrasonic nano particle dispersion reactor in a kind of gas-lifting type |
| CN111007153A (en) * | 2018-10-08 | 2020-04-14 | 浙江大学 | Detection method for gas-liquid dispersion state of jet bubbling reactor |
| CN111007153B (en) * | 2018-10-08 | 2020-10-30 | 浙江大学 | Detection method for gas-liquid dispersion state of jet bubbling reactor |
| CN111036149A (en) * | 2019-12-02 | 2020-04-21 | 河南金鹏化工有限公司 | Water-washing continuous production process and device for thiodicarb |
| CN111036149B (en) * | 2019-12-02 | 2023-06-23 | 河南金鹏化工有限公司 | Thiodicarb water washing continuous production process and device |
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Application publication date: 20091202 |