CN203448075U - Gas-liquid double-circulation reaction device for preparing glyoxylic acid by utilizing air oxidation method - Google Patents
Gas-liquid double-circulation reaction device for preparing glyoxylic acid by utilizing air oxidation method Download PDFInfo
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- CN203448075U CN203448075U CN201320527197.5U CN201320527197U CN203448075U CN 203448075 U CN203448075 U CN 203448075U CN 201320527197 U CN201320527197 U CN 201320527197U CN 203448075 U CN203448075 U CN 203448075U
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Abstract
The utility model discloses a gas-liquid double-circulation reaction device for preparing glyoxylic acid by utilizing an air oxidation method. The gas-liquid double-circulation reaction device comprises a reaction kettle (6), a stirring paddle (7), a discharge valve (8), a heating steam valve (5) and a lower cooling water valve (9). The gas-liquid double-circulation reaction device is characterized in that the reaction kettle (6) is additionally provided with a kettle liquid circulation absorption device and an air current circulation device; without changing of the existing equipment arrangement of a producing department, glyoxal can be oxidized into a glyoxylic acid product by using nitric oxide which is generated in the process of oxidizing glyoxal with nitric acid as a catalyst and using oxygen in the air as an oxidizing agent. The gas-liquid double-circulation reaction device disclosed by the utility model has the advantages that the structure is reasonable, the operation is simple, the cost is saved, the use is safe and the like, the consumption of a nitric acid is greatly reduced, the NOX tail gas discharge value is also reduced, and the yield of a product glyoxylic acid is also improved.
Description
One, technical field
The utility model belongs to medication chemistry production field, relates in particular to the two circular response devices of gas-liquid that a kind of air oxidation process is prepared glyoxalic acid.
Two, background technology
Glyoxalic acid, OHC-COOH, has the character of aldehyde and carboxylic acid concurrently, is a kind of important chemical intermediate and biochemical reagents.By glyoxalic acid, can derive tens kinds of details chemical products, be widely used in the fields such as medicine, spices, agricultural chemicals, paint, papermaking, food additives.
Enterprise produces the common production technology adopting of glyoxalic acid: nitric acid oxidation glyoxal method.Patent CN200710054917.X, by using acidic catalyst (example hydrochloric acid), has solved the problem that glyoxal oxidizing process Raw gathers and reaction sets off an explosion suddenly.But the method is also deposited and is produced in process of production a large amount of NO
xtail gas, the problem such as contaminated environment and nitric acid consumption are large.Patent CN102247748A, introduces air the NO in glyoxal nitric acid oxidation generation tail gas is oxidized to NO
2; Water carries out after 6 grades of absorptions, with alkali liquor absorption, and absorption liquid is processed to rear section recycled.But the method also exists nitric acid consumption large, the problem such as the large and absorption equipment of vent gas treatment amount is huge.Patent CN102553628A, take vanadic anhydride as catalyst, take airborne oxygen as oxidant, overcome the large shortcoming of traditional preparation method's environmental pollution, but catalyst preparation cost is high.
Three, summary of the invention
The purpose of this utility model is exactly that a kind of to take the nitrogen oxide producing in nitric acid oxidation glyoxal process be catalyst in order to provide, and the air oxidation process that the airborne oxygen of take is oxidant is prepared the two circular response devices of gas-liquid of glyoxalic acid.
The technical scheme that the utility model adopts is: it is reactor, paddle, outlet valve, heating steam valve and lower cooling water valve etc., to consist of on conventional production equipment basis, setting up still liquid circulation absorption plant and air current circulation on reactor.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, shower nozzle are established in top, and blast pipe is established on top; Described air current circulation is comprised of gas circulation blower fan, gas flow regulating valve air distributor and pipeline, the inlet pipeline of gas circulation blower fan is communicated with reactor upper gas, and its port of export joins with the pipeline with gas flow regulating valve and 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.Heating steam valve and boiler steam pipeline on reactor join, and cooling water valve is connected with cooling water pipeline, and the air inlet with volume damper is established at reactor top, Gas Stirring blade is established on top, liquid agitation blade is established in bottom, approaches bottom and establishes air distributor, and outlet valve is established in bottom.
The beneficial effects of the utility model are: on the basis of original produces tartronic device, only need set up still liquid circulation absorption plant and air current circulation, do not need to change workshop existing equipment layout, just can directly utilize original reactor, the nitrogen oxide producing in nitric acid oxidation glyoxal process of take is catalyst, with airborne oxygen, make oxidant, 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, and 3 is frequency converter, and 4 is air flow rate adjustment valve, 5 is heating steam valve, and 6 is reactor, and 7 is paddle, and 8 is outlet valve, 9 is lower cooling water valve, and 10 is Gas Stirring blade, and 11 is return bend, and 12 is gas pipeline, 13 is absorbing column, and 14 is cooling tube, and 15 is shower nozzle, and 16 is blast pipe, 17 is lower charging aperture, and 18 is filler, and 19 is upper cooling water valve, 20 is air distributor, and 21 is gas flow regulating valve, and 22 is blower fan.
Five, the specific embodiment
As shown in Figure 1, on the basis of original produces tartronic device technique equipment, air current circulation and and air current circulation have been set up.Described still liquid circulation absorption plant is by being connected with reactor 6 with gas pipeline 12 by return bend 11 and side's placed on it absorbing column 13, pump 2 and frequency converter 3 form, the entrance point of pump 2 is connected with the pipeline in inserting reactor 6 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 13 bottoms, cooling tube 14, shower nozzle 15 are established in top, and blast pipe 16 is established on top.Described air current circulation is comprised of gas circulation blower fan 22, gas flow regulating valve 21 air distributors 20 and pipeline, the inlet pipeline of gas circulation blower fan 20 is communicated with reactor 6 upper gas, its port of export joins with the pipeline with gas flow regulating valve 21 and the air distributor 20 that is arranged at still inner bottom part, and 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, and drips rare nitric acid complete, drips 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 ℃, stop 40% nitric acid dropping, if still temperature continues to rise, open large lower cooling water valve; If below still temperature drop to 59 ℃, 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 (3)
1. an air oxidation process is prepared the two circular response devices of gas-liquid of glyoxalic acid, it comprises reactor (6), paddle (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 and air current circulation.
2. air oxidation process according to claim 1 is prepared the two circular response devices of gas-liquid of glyoxalic acid, it is characterized in that: 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 (6) 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 (13) bottom, cooling tube (14) is established on top, shower nozzle (15), blast pipe (16) is established on top, described air current circulation is comprised of gas circulation blower fan (22), gas flow regulating valve (21) air distributor (20) and pipeline, the inlet pipeline of gas circulation blower fan (20) is communicated with reactor (6) upper gas, its port of export joins with the air distributor (20) that is arranged at still inner bottom part with the pipeline of band gas flow regulating valve (21), and 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).
3. air oxidation process according to claim 2 is prepared the two circular response devices of gas-liquid of glyoxalic acid, it is characterized in that: described air distributor (20) is disc, and is provided with venthole at its surface uniform.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320527197.5U CN203448075U (en) | 2013-08-28 | 2013-08-28 | Gas-liquid double-circulation reaction device for preparing glyoxylic acid by utilizing air oxidation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320527197.5U CN203448075U (en) | 2013-08-28 | 2013-08-28 | Gas-liquid double-circulation reaction device for preparing glyoxylic acid by utilizing air oxidation method |
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| CN201320527197.5U Expired - Fee Related CN203448075U (en) | 2013-08-28 | 2013-08-28 | Gas-liquid double-circulation reaction device for preparing glyoxylic acid by utilizing air oxidation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2013
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
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Legal Events
| Date | Code | Title | Description |
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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: 20140226 Termination date: 20140828 |
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| EXPY | Termination of patent right or utility model |