CN203700236U - Device for preparing glyoxylic acid by using normal pressure air oxidation method and adopting cold residue to absorb tail gas - Google Patents
Device for preparing glyoxylic acid by using normal pressure air oxidation method and adopting cold residue to absorb tail gas Download PDFInfo
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- CN203700236U CN203700236U CN201420049343.2U CN201420049343U CN203700236U CN 203700236 U CN203700236 U CN 203700236U CN 201420049343 U CN201420049343 U CN 201420049343U CN 203700236 U CN203700236 U CN 203700236U
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Abstract
The utility model discloses a device for preparing glyoxylic acid by using a normal pressure air oxidation method and adopting cold residue to absorb tail gas, and solves problems that requirements on equipment are higher, the cost is higher, the operation is more difficult and the separation of inert gas and nitrogen oxide in the air is difficult in the prior art. The device is characterized in that on the basis of original glyoxylic acid production technical equipment which adopts a nitric acid oxidation method and is provided with a tail gas treatment system, a gas-liquid spraying and mixing circular reaction device, a tail gas circulation absorbing device by using cold residue and a liquid seal alarming device are additionally arranged. By the adoption of the device, the consumption of nitric acid is greatly reduced, pure oxygen raw material is not needed, and glyoxylic acid can be prepared by only using oxygen in the air to oxidize glyoxal.
Description
One, technical field
The utility model belongs to chemical reaction equipment, relates to a kind of cold still liquid absorption tail gas atmospheric air oxidation style and prepares oxoethanoic acid device.
Two, background technology
Oxoethanoic acid (OHC-COOH), having another name called gyloxylic acid, GA, is the simplest aldehydic acid of one, has the character of acid and aldehyde concurrently, be a kind of important industrial chemicals and intermediate, be mainly used in the fields such as medicine, agricultural chemicals, spices, foodstuff additive, biological chemistry.Along with the development in oxoethanoic acid derived product market, it has become large Chemicals that industrial scale reaches tens thousand of tons, and market requirement steady-state growth.
At present, oxoethanoic acid industrialized preparing process can be divided into chemical synthesis and the large class of electrochemical synthesis two, industrial the most frequently used chemical synthesis mainly contains two kinds of oxoethanoic acid nitric acid oxidation method and toxilic acid (acid anhydride) Ozonations, and electrochemical synthesis comprises acid by electrolytic reduction of oxalic method and Ethanedial electrolyzing and oxidizing method etc.Wherein, oxalic dialdehyde nitric acid oxidation method is through improvement for many years, its reaction conditions gentleness, and technique is simply ripe, and raw material is cheap and easy to get, and production cost is low, is the most general Synthetic Methods of Glyoxalic Acid of manufacturer's application both at home and abroad at present.But this method is also deposited and is produced in process of production a large amount of NO
xtail gas, the problem such as contaminate environment and nitric acid consumption are large.For how effectively reducing NO
xtail gas pollution, in the existing way of chemosynthesis technical field as patent of invention " technology for absorbing tail gas of glyoxalic acid production ", 200810049919.4, Xie Jianzhong.Adopt three grades of absorption units to absorb, front I and II is absorbing pure water, and the third stage is that 10-20% sodium hydroxide solution absorbs.And for example patent of invention " a kind of oxalic dialdehyde nitric acid oxidation method is produced exhaust gas treating method and the treatment system of oxoethanoic acid ", 201110185138.X, Bao Yingyuan.The NO that introducing air produces oxalic dialdehyde nitric acid oxidation in tail gas is oxidized to NO2, and water carries out after 6 grades of absorptions, with alkali liquor absorption, and absorption liquid is processed to rear section recycled.But aforesaid method also exists nitric acid consumption large, the problem such as the large and absorption equipment of vent gas treatment amount is huge.How to reduce nitric acid consumption, existing way is as patent of invention " synthetic method of preparing glyoxalic acid solution by oxygen catalytic oxidation of glyoxal with nitrogen oxide ", 200410096499.7, Zhou Zhiming.And for example patent of invention " preparing the method for aqueous glyoxylic acid ", 200980102995.X, F Donald Bragg.They are in closed reactor, and the nitrogen oxide catalysis producing with nitric acid oxidation oxalic dialdehyde is used dioxygen oxidation glyoxal water solution to prepare aqueous glyoxylic acid.Aforesaid method is to carry out in encloses container, can gather because of raw material, react and set off an explosion suddenly, has very large potential safety hazard.With the comparison of traditional nitric acid oxidation oxalic dialdehyde method, its equipment requirements is higher, and equipment cost increases, and operation easier increases; Although saved nitric acid, increase the not low purity oxygen of price.If with inexhaustible, the oxygen-containing gas air that need not spend, just needs the reactor that volume is larger, will further increase equipment cost, or solves the separation problem of airborne rare gas element and nitrogen oxide.
Three, summary of the invention
The purpose of this utility model is exactly in order to provide a kind of under original synthesis under normal pressure appointed condition, both reduced nitric acid consumption, also without pure oxygen raw material, realize industrialized cold still liquid absorption tail gas atmospheric air oxidation style by the method for the dioxygen oxidation glyoxal preparation oxoethanoic acid in nitrogen oxide catalytic air and prepare oxoethanoic acid device.
The technical scheme that the utility model adopts is: this device comprises the facilities such as reactor, liquid pump, air pump, gas-liquid injection mixing tank, absorption column and liquid seal trough, on the basis of the nitric acid oxidation method produces tartronic device technique equipment of original hot tail gas treatment system, set up gas-liquid injection mixed cycle reaction unit, cold still liquid circulation absorbs tail gas unit and fluid-tight warning device.Described gas-liquid injection mixed cycle reaction unit is made up of air pump, air pump frequency transformer, gas-liquid injection mixing tank and pipeline, the inlet pipeline of air pump is communicated with reactor upper gas, its exit end is connected with the gas inlet tube of gas-liquid injection mixing tank, the liquid inlet tube of gas-liquid injection mixing tank is connected with Polycondensation Reactor and Esterification Reactor discharge nozzle or directly at the bottom of insertion reaction still, gas-liquid mixture fluid outlet pipe is communicated with reactor top, it is existing multistage water to be absorbed to last in tail gas unit change into cold still liquid circulation absorption tail gas to what that described cold still liquid circulation absorbs tail gas unit, by being connected with reactor with gas pipeline by return bent pipe and side's placed on it absorption column, liquid pump and liquid pump frequency transformer composition, the entrance end of liquid pump is connected with the pipeline in insertion reaction still liquid, its exit end is connected with one end of spiral coil cooling tube in water cooler by transport pipe, the other end of spiral coil cooling tube is connected with the shower nozzle being arranged in absorption column, cooling water valve is established in water cooler bottom, cooling water overflow pipe is established on top, filler is established in absorption column inside, top is established vapor pipe and is communicated with tail gas bottle, the air intlet pipe of magnetic tape trailer gas cylinder pressure lock is established in tail gas bottle side, the offgas duct of the Flash Gas Compression Skid System that truncates is established at top, described fluid-tight warning device is to be connected with the liquid seal trough that warning howler is housed by pipeline by the vapor pipe that is arranged on reactor top.Heating steam valve and boiler steam pipeline on reactor join, and lower cooling water valve is connected with cooling water pipeline, and the air intlet pipe with reactor pressure lock is established at reactor top, and bleeder valve is established in bottom, and gas stirring blade is established on top, and liquid agitation blade is established in bottom.
Compared with prior art, tool has the following advantages and beneficial effect the utility model: the dioxygen oxidation method in air that realized is carried out in normal-pressure reaction kettle, has saved facility investment, has reduced operation easier, has increased safety coefficient; Compared with traditional nitric acid oxidation method, both greatly reduced the consumption of nitric acid, also greatly reduce NO
xexhaust emissions amount, has also improved the yield of product oxoethanoic acid.
Below in conjunction with accompanying drawing, the utility model is described in further detail:
Four, accompanying drawing explanation:
Fig. 1 is structural principle schematic diagram of the present utility model.
In figure: 1 is upper feeding mouth, 2 is liquid pump, 3 is liquid pump frequency transformer, 4 is lower opening for feed, 5 is heating steam valve, 6 is lower cooling water valve, 7 is reactor, 8 is bleeder valve, 9 is outlet valve, 10 is liquid agitation blade, 11 is gas stirring blade, 12 is gas-liquid injection mixing tank, 13 is reactor pressure lock, 14 is air pump frequency transformer, 15 is air pump, 16 is return bent pipe, 17 is gas pipeline, 18 is filler, 19 is absorption column, 20 is shower nozzle, 21 is offgas duct, 22 is tail gas bottle pressure lock, 23 is tail gas bottle, 24 is water cooler, 25 is upper cooling water valve, 26 is warning howler, 27 is liquid seal trough.
Five, embodiment
As shown in Figure 1, on the basis of the nitric acid oxidation method produces tartronic device technique equipment of original hot tail gas treatment system, set up gas-liquid injection mixed cycle reaction unit, cold still liquid circulation absorbs tail gas unit and fluid-tight warning device.Described gas-liquid injection mixed cycle reaction unit is made up of air pump 15, air pump frequency transformer 14, gas-liquid injection mixing tank 12 and pipeline, the inlet pipeline of air pump 15 is communicated with reactor 7 upper gas, its exit end is connected with the gas inlet tube of gas-liquid injection mixing tank 12, the liquid inlet tube of gas-liquid injection mixing tank 12 is connected with 7 end of reactor discharge nozzle or direct 7 ends of insertion reaction still, and gas-liquid mixture fluid outlet pipe is communicated with reactor 7 tops, it is that return bent pipe 16 is connected with reactor 7 with gas pipeline and side's placed on it absorption column 19 by passing through that described cold still liquid circulation absorbs tail gas unit, liquid pump 2 and liquid pump frequency transformer 3 form, the entrance end of liquid pump 2 is connected with the pipeline in insertion reaction still 7 liquid, its exit end is connected with one end of water cooler 24 interior spiral coil cooling tubes by transport pipe, the other end of spiral coil cooling tube is connected with the shower nozzle 20 being arranged in absorption column 19, cooling water valve 25 is established in water cooler 24 bottoms, cooling water overflow pipe is established on top, filler 18 is established in absorption column 19 inside, top is established vapor pipe and is communicated with tail gas bottle 23, the air intlet pipe of magnetic tape trailer gas cylinder pressure lock 22 is established in tail gas bottle 23 sides, the offgas duct 21 of the Flash Gas Compression Skid System that truncates is established at top, described fluid-tight warning device is to be connected with the liquid seal trough 27 that warning howler 26 is housed by pipeline by the vapor pipe that is arranged on reactor 7 tops.Heating steam valve 5 on reactor 7 joins with boiler steam pipeline, lower cooling water valve 6 is connected with cooling water pipeline, and the air intlet pipe with reactor pressure lock 13 is established at reactor 7 tops, and bleeder valve 8 is established in bottom, gas stirring blade 11 is established on top, and liquid agitation blade 10 is established in bottom.
While implementing the utility model, a certain amount of 20-40% glyoxal solution is added in reactor 7, appropriate technical hydrochloric acid and water are dropped into reactor 7, under stirring, crack heating steam valve 5, while being slowly warming up to 55 ℃, cuts out heating steam valve 5.Drip rare nitric acid that appropriate water absorbs tail gas gained, reaction starts immediately, there is reddish-brown NO gas to emit, drip rare nitric acid complete, drip immediately 40% nitric acid preparing in advance, when temperature rises to 60 ℃, open cooling water valve 6, open exhaust fan, reactor pressure lock 13, tail gas bottle pressure lock 22, upper cooling water valve 25 and liquid pump 2, increase gradually air pump 15 frequencies to definite value, reduce gradually and drip 40% nitric acid to stopping, maintain temperature of reaction at 55-65 ℃, reaction pressure is normal pressure, when system positive pressure alarm equipment alarm or temperature exceed 61 ℃, increase lower cooling water flow or reduce air pump 15 frequencies, when system negative pressure alarm equipment alarm or temperature drop to below 59 ℃, reduce lower cooling water flow, increase air pump 15 frequencies or drip nitric acid supplemental nitrogen, in the time that tail gas bottle 23 has reddish-brown NO gas, the frequency that increases liquid pump 2 disappears to reddish-brown, in the time dripping oxygen sum that the nitric acid oxygen of emitting and air bring into reach chemical reaction point of equivalent in oxidation reaction process, stop logical oxygen, insulation reaction 1 hour, is cooled to 0-5 ℃, separates out white crystal, filters to obtain oxalic acid, and filtrate is glyoxylic acid solution.
Claims (3)
1. a cold still liquid absorption tail gas atmospheric air oxidation style is prepared oxoethanoic acid device, it comprises reactor (7), liquid pump (2), air pump (15), gas-liquid injection mixing tank (12), absorption column (19) and liquid seal trough (27), it is characterized in that: described gas-liquid injection mixed cycle reaction unit is by air pump (15), air pump frequency transformer (14), gas-liquid injection mixing tank (12) and pipeline composition, the inlet pipeline of air pump (15) is communicated with reactor (7) upper gas, its exit end is connected with the gas inlet tube of gas-liquid injection mixing tank (12), the liquid inlet tube of gas-liquid injection mixing tank (12) is connected with reactor (7) end discharge nozzle or direct insertion reaction still (7) end, gas-liquid mixture fluid outlet pipe is communicated with reactor (7) top.
2. the cold still liquid absorption of one according to claim 1 tail gas atmospheric air oxidation style is prepared oxoethanoic acid device, it is characterized in that: it is that return bent pipe (16) is connected with reactor (7) with gas pipeline and side's placed on it absorption column (19) by passing through that described cold still liquid circulation absorbs tail gas unit, liquid pump (2) and liquid pump frequency transformer (3) composition, the entrance end of liquid pump (2) is connected with the pipeline in insertion reaction still (7) liquid, its exit end is connected with one end of the interior spiral coil cooling tube of water cooler (24) by transport pipe, the other end of spiral coil cooling tube is connected with the shower nozzle (20) being arranged in absorption column (19), cooling water valve (25) is established in water cooler (24) bottom, cooling water overflow pipe is established on top, filler (18) is established in absorption column (19) inside, top is established vapor pipe and is communicated with tail gas bottle (23), the air intlet pipe of magnetic tape trailer gas cylinder pressure lock (22) is established in tail gas bottle (23) side, the offgas duct (21) of the Flash Gas Compression Skid System that truncates is established at top.
3. the cold still liquid absorption of one according to claim 1 tail gas atmospheric air oxidation style is prepared oxoethanoic acid device, it is characterized in that: described fluid-tight warning device is to be connected with the liquid seal trough (27) that warning howler (26) are housed by pipeline by the vapor pipe that is arranged on reactor (7) top; Heating steam valve (5) on reactor (7) joins with boiler steam pipeline, lower cooling water valve (6) is connected with cooling water pipeline, the air intlet pipe of band reactor pressure lock (13) is established at reactor (7) top, bleeder valve (8) is established in bottom, gas stirring blade (11) is established on top, and liquid agitation blade (10) is established in bottom.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420049343.2U CN203700236U (en) | 2014-01-18 | 2014-01-18 | Device for preparing glyoxylic acid by using normal pressure air oxidation method and adopting cold residue to absorb tail gas |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420049343.2U CN203700236U (en) | 2014-01-18 | 2014-01-18 | Device for preparing glyoxylic acid by using normal pressure air oxidation method and adopting cold residue to absorb tail gas |
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| CN203700236U true CN203700236U (en) | 2014-07-09 |
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| CN201420049343.2U Expired - Fee Related CN203700236U (en) | 2014-01-18 | 2014-01-18 | Device for preparing glyoxylic acid by using normal pressure air oxidation method and adopting cold residue to absorb tail gas |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2014
- 2014-01-18 CN CN201420049343.2U patent/CN203700236U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
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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: 20140709 Termination date: 20160118 |
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| EXPY | Termination of patent right or utility model |