CN203525676U - Gas-liquid double-cycle reaction device for preparing glyoxylic acid by using oxygen oxidation method - Google Patents
Gas-liquid double-cycle reaction device for preparing glyoxylic acid by using oxygen oxidation method Download PDFInfo
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- CN203525676U CN203525676U CN201320734501.3U CN201320734501U CN203525676U CN 203525676 U CN203525676 U CN 203525676U CN 201320734501 U CN201320734501 U CN 201320734501U CN 203525676 U CN203525676 U CN 203525676U
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Abstract
The utility model discloses a gas-liquid double-cycle reaction device for preparing glyoxylic acid by using an oxygen oxidation method. The device is used for solving the problems that plenty of nitrogen oxide is generated, the environment is seriously polluted and the like in the prior art. The device is characterized in that a kettle residue circular absorbing device, an air flow circulating device and a liquid seal warning device are additionally arranged on a reaction kettle (6); the kettle residue circular absorbing device comprises an absorbing column (13), a pump (2) and a frequency converter (3) which are connected with the reaction kettle (6) through a return bent pipe (11) and a gas pipeline (12) and arranged above the reaction kettle; the air flow circulating device comprises a gas circulating fan (22), a gas flow adjusting valve (21), a gas mixer (23), a gas flow distributor (20), a measurement scale (25), an oxygen adjusting valve (24) and pipelines. The reaction device has the advantages of reasonable structure, simplicity in operation, cost reduction, safety in use and the like and has the benefits of greatly reducing the consumption of nitric acid, reducing the emission of NOX tail gas and increasing the yield of the product glyoxylic acid.
Description
One, technical field
The utility model belongs to field of medicine and chemical technology, relates in particular to a kind of dioxygen oxidation legal system for the two circular response devices of gas-liquid of glyoxalic acid.
Two, background technology
Glyoxalic acid is a kind of important industrial chemicals, and its skeleton symbol is OHC-COOH, can be used for preparing the products such as allantoin, vanillic aldehyde, Amoxicillin.
The preparation method that glyoxalic acid is conventional has nitric acid oxidation method, dioxygen oxidation method, hydrogen peroxide method, electrochemical process etc.Zhang Kefeng, modern chemical industry, 1992(4) has reported in 62-63 that the method is the main method of current industrial production glyoxalic acid by the method for nitric acid oxidation glyoxal preparation glyoxalic acid, but its course of reaction produces with a large amount of nitrogen oxide, and environmental pollution is serious.Patent CN102553628A, take vanadic anhydride as catalyst, take airborne oxygen as oxidant, overcome the large shortcoming of nitric acid oxidation method environmental pollution, but catalyst preparation cost is high.200410096499.7, Zhou Zhiming.It is in closed reactor, and with in nitric acid oxidation glyoxal process, the nitrogen oxide oxygen catalytic oxidation glyoxal water solution of generation is prepared glyoxalic acid solution.This method has solved the high problem of catalyst cost, but its requirement autoclave increases equipment cost; Under high-pressure sealed state, operate, potential safety hazard is increased; Only under laboratory condition, complete experiment, do not solve mass transfer and heat transfer problem in industrial amplification process, so far still unrealized industrialization.
Three, summary of the invention
The purpose of this utility model is exactly that a kind of reasonable in design, consumption of raw materials amount are few in order to provide, safety environment protecting energy saving take dioxygen oxidation legal system that the nitrogen oxide that produces in nitric acid oxidation glyoxal process the is catalyst two circular response devices of gas-liquid for glyoxalic acid.
The technical scheme that the utility model adopts is: it is by reactor, stirring arm, outlet valve, in the conventional production equipment that heating steam valve and lower cooling water valve etc. form, set up still liquid circulation absorption plant, air current circulation and fluid-tight warning device, described still liquid circulation absorption plant is by being connected with reactor with gas pipeline by return bend and side's placed on it absorbing column, pump and frequency converter form, the entrance point of pump is connected with the pipeline in inserting reactor liquid by communicating valve, its port of export is connected with the shower nozzle in being arranged at absorbing column by conveyance conduit, filler is established in absorbing column bottom, cooling tube and shower nozzle are established in top, exhaust outlet is established on top, by pipeline, be connected with the liquid seal trough that alarm is housed, described air current circulation is comprised of gas circulation blower fan, gas flow regulating valve, gas mixer, air distributor, weigher, oxygen regulating valve and pipeline, the inlet pipeline of gas circulation blower fan is communicated with absorbing column top discharge duct, its port of export is connected with gas mixer, the oxygen bottle being placed on weigher is connected with gas mixer by the pipeline of gas gas control valve is set, and the mixed gas outlet pipeline of gas mixer joins with the air distributor that is arranged at still inner bottom part, on the kettle cover of reactor, being provided with bottom has liquid agitation oar, top to have the shaft of Gas Stirring blade.Described air distributor is disc, and is provided with venthole at its surface uniform.
The beneficial effects of the utility model are: adopt still liquid circulation absorption plant and air current circulation, the nitrogen oxide producing in nitric acid oxidation glyoxal process of take is catalyst, with airborne oxygen, makes oxidant, and glyoxal is oxidized to glyoxalic acid product.There is the advantages such as rational in infrastructure, simple to operate, cost-saving, use is safe, both greatly reduced the consumption of nitric acid, also reduced NO
xexhaust emissions amount, has also improved the yield of product glyoxalic acid.
Below in conjunction with accompanying drawing, the utility model is described in further detail.
Four, accompanying drawing explanation:
Fig. 1 is structural representation of the present utility model.
In figure: 1 is upper feeding mouth, 2 is pump, 3 is frequency converter, 4 is atmospheric valve, 5 is heating steam valve, 6 is reactor, 7 is paddle, 8 is outlet valve, 9 is lower cooling water valve, 10 is Gas Stirring blade, 11 is return bend, 12 is gas pipeline, 13 is absorbing column, 14 is cooling tube, 15 is shower nozzle, 16 is blast pipe, 17 is lower charging aperture, 18 is filler, 19 is upper cooling water valve, 20 is air distributor, 21 is recyclegas flow control valve, 22 is blower fan, 23 is gas mixer, 24 is oxygen regulating valve, 25 is weigher, 26 is alarm, 27 is liquid seal trough.
Five, the specific embodiment
As shown in Figure 1, it is with reactor 6, stirring arm 7, outlet valve 8, what heating steam valve 5 and lower cooling water valve 9 etc. formed produces on the production equipment basis of glyoxalic acid with nitric acid oxidation glyoxal, set up still liquid circulation absorption plant, air current circulation and fluid-tight warning device, described still liquid circulation absorption plant is that return bend 11 is connected with reactor 6 with gas pipeline 12 and side's placed on it absorbing column 13 by passing through, pump 2 and frequency converter 3 form, the entrance point of pump 2 is connected with the pipeline in inserting reactor liquid by communicating valve, its port of export is connected with the shower nozzle 15 in being arranged at absorbing column 13 by conveyance conduit, filler 18 is established in absorbing column bottom, cooling tube 14 and shower nozzle 15 are established in top, exhaust outlet is established on top, by pipeline 16, be connected with the liquid seal trough 27 that alarm 26 is housed, described air current circulation is comprised of gas circulation blower fan 22, gas flow regulating valve 21, gas mixer 23, air distributor 20, weigher 25, oxygen regulating valve 24 and pipeline, the inlet pipeline of gas circulation blower fan 22 is communicated with absorbing column top discharge duct 16, its port of export is connected with gas mixer 23, the oxygen bottle being placed on weigher 25 is connected with gas mixer 23 by the pipeline of gas gas control valve 24 is set, and the mixed gas outlet pipeline of gas mixer 23 joins with the air distributor 20 that is arranged at still inner bottom part, on the kettle cover of reactor 6, being provided with bottom has liquid agitation oar 7, top to have the shaft of Gas Stirring blade 10.Described air distributor 20 is disc, and is provided with venthole at its surface uniform.While implementing the utility model, a certain amount of 20-40% glyoxal solution is added reactor 6 from upper feeding mouth 1, appropriate technical hydrochloric acid and water are dropped into reactor from lower charging aperture 17, under stirring, crack heating steam valve 5, while being slowly warming up to 55 ℃, cuts out heating steam valve 5.Then start circulating pump 2, in unlatching, cooling water valve 19, and drip rare nitric acid that appropriate water absorbs tail gas gained, and reaction starts immediately, has rufous NO
xgas is emitted, drip rare nitric acid complete, drip immediately 40% nitric acid preparing in advance, when temperature rises to 59 ℃, open lower cooling water valve 9, reduce by 40% nitric acid dropping speed, start gas circulation blower fan 2, adjusting gas flow control valve 21, to the similar fluidized state of still liquid, starts tail gas outlet blower fan, and air flow rate adjustment valve 4 is opened to tail gas outlet and discharges without obvious yellow gas, when temperature surpasses 61 ℃ or high pressure alarm report to the police, stop 40% nitric acid dropping, if still temperature continues to rise, open large lower cooling water valve; If still temperature drop to 59 ℃ following or low pressure alarm warning, turn or close lower cooling water valve down, if still temperature continues to decline, drip in right amount 40% nitric acid, maintain reaction temperature at 55-65 ℃, when dripping the oxygen that nitric acid emits in oxidation reaction process and pass into oxygen sum that air brings into while surpassing reaction equivalent point certain value, stop gas circulation, insulation reaction 1 hour, be cooled to 0-5 ℃, separate out white crystal, filter to obtain oxalic acid, filtrate is glyoxylic acid solution.
Claims (2)
1. a dioxygen oxidation legal system is for the two circular response devices of gas-liquid of glyoxalic acid, it comprises reactor (6), stirring arm (7), outlet valve (8), heating steam valve (5) and lower cooling water valve (9), it is characterized in that: on reactor (6), set up still liquid circulation absorption plant, air current circulation and fluid-tight warning device, described still liquid circulation absorption plant is that return bend (11) is connected with reactor (6) with gas pipeline (12) and side's placed on it absorbing column (13) by passing through, pump (2) and frequency converter (3) form, the entrance point of pump (2) is connected with the pipeline in inserting reactor liquid by communicating valve, its port of export is connected with the shower nozzle (15) in being arranged at absorbing column (13) by conveyance conduit, filler (18) is established in absorbing column bottom, cooling tube (14) and shower nozzle (15) are established in top, exhaust outlet is established on top, by pipeline (16), be connected with the liquid seal trough (27) that alarm (26) are housed, described air current circulation is by gas circulation blower fan (22), gas flow regulating valve (21), gas mixer (23), air distributor (20), weigher (25), oxygen regulating valve (24) and pipeline form, the inlet pipeline of gas circulation blower fan (22) is communicated with absorbing column top discharge duct (16), its port of export is connected with gas mixer (23), the oxygen bottle being placed on weigher (25) is connected with gas mixer (23) by the pipeline of gas gas control valve (24) is set, the mixed gas outlet pipeline of gas mixer (23) joins with the air distributor (20) that is arranged at still inner bottom part, on the kettle cover of reactor (6), being provided with bottom has liquid agitation oar (7), top to have the shaft of Gas Stirring blade (10).
2. dioxygen oxidation legal system according to claim 1, for the two circular response devices of gas-liquid of glyoxalic acid, is characterized in that: described air distributor (20) is disc, and is provided with venthole at its surface uniform.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320734501.3U CN203525676U (en) | 2013-11-20 | 2013-11-20 | Gas-liquid double-cycle reaction device for preparing glyoxylic acid by using oxygen oxidation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320734501.3U CN203525676U (en) | 2013-11-20 | 2013-11-20 | Gas-liquid double-cycle reaction device for preparing glyoxylic acid by using oxygen oxidation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106166470A (en) * | 2016-07-23 | 2016-11-30 | 河南新天地药业股份有限公司 | A kind of dynamic hydraulic combined reaction unit |
| CN109280004A (en) * | 2018-11-30 | 2019-01-29 | 黄冈师范学院 | The method, apparatus and application of nitrogen oxide catalytic air oxidation glyoxal glyoxalic acid |
| CN109319776A (en) * | 2018-11-30 | 2019-02-12 | 黄冈师范学院 | The method, apparatus and application of nitrogen oxide and iron ion catalysis oxidation recycling diamond |
| CN110270297A (en) * | 2019-07-31 | 2019-09-24 | 河南新天地药业股份有限公司 | A kind of tower reactor of synthesizing glyoxalic acid |
-
2013
- 2013-11-20 CN CN201320734501.3U patent/CN203525676U/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106166470A (en) * | 2016-07-23 | 2016-11-30 | 河南新天地药业股份有限公司 | A kind of dynamic hydraulic combined reaction unit |
| CN109280004A (en) * | 2018-11-30 | 2019-01-29 | 黄冈师范学院 | The method, apparatus and application of nitrogen oxide catalytic air oxidation glyoxal glyoxalic acid |
| CN109319776A (en) * | 2018-11-30 | 2019-02-12 | 黄冈师范学院 | The method, apparatus and application of nitrogen oxide and iron ion catalysis oxidation recycling diamond |
| CN109280004B (en) * | 2018-11-30 | 2023-08-22 | 黄冈师范学院 | Method, device and application for preparing glyoxalic acid by oxidizing glyoxal through nitrogen oxide catalysis air |
| CN109319776B (en) * | 2018-11-30 | 2023-09-15 | 黄冈师范学院 | Method, device and application for recycling diamond through catalytic oxidation of nitrogen oxide and iron ions |
| CN110270297A (en) * | 2019-07-31 | 2019-09-24 | 河南新天地药业股份有限公司 | A kind of tower reactor of synthesizing glyoxalic acid |
| CN110270297B (en) * | 2019-07-31 | 2024-02-06 | 新天地药业股份有限公司 | Tower reactor for synthesizing glyoxylic acid |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140409 Termination date: 20141120 |
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| EXPY | Termination of patent right or utility model |