CN205032176U - Oxidation reaction unit of glyoxalic acid - Google Patents
Oxidation reaction unit of glyoxalic acid Download PDFInfo
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- CN205032176U CN205032176U CN201520778036.2U CN201520778036U CN205032176U CN 205032176 U CN205032176 U CN 205032176U CN 201520778036 U CN201520778036 U CN 201520778036U CN 205032176 U CN205032176 U CN 205032176U
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- Prior art keywords
- tail gas
- anger
- reactor
- absorbing liquid
- gas condenser
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses an oxidation reaction unit of glyoxalic acid, including reation kettle, tail gas condenser, reation kettle and tail gas condenser link to each other through the back flow of giving vent to anger, the back flow of giving vent to anger still is equipped with the sealed tube outward, it forms confined space to give vent to anger between the inner wall of outer wall and the sealed tube of back flow, still be connected with the breathing pipe with the confined space intercommunication on the pipe wall of sealed tube, the other end and the vacuum pump connection of breathing pipe, through setting up the sealed tube outside the backflow pipeline that gives vent to anger, then through breathing pipe and vacuum pump, can be with giving vent to anger confined space vacuum production state between back flow and the sealed tube, when the condensate of the tail gas that comes out from the reation kettle and backward flow from the tail gas condenser through giving vent to anger the back flow when, because its outside is the vacuum state, so avoided the externally to corrode the risk of the back flow of giving vent to anger, its stability in use has been strengthened.
Description
Technical field
The utility model relates to chemical reaction device field, in particular, relates to a kind of oxidation reaction apparatus of glyoxalic acid.
Background technology
Glyoxalic acid is a kind of important fine chemical material and intermediate, is widely used in the synthesis field of the light industrial goods such as spices, medicine, agricultural chemicals, papermaking, coating, paint, leather and food additives.At present, industrial comparatively conventional chemical synthesis process mainly contains glyoxal nitric acid oxidation method, acid by electrolytic reduction of oxalic method, maleic acid (acid anhydride) Ozonation three kinds.Wherein, glyoxal nitric acid oxidation method, with its lower cost and more ripe technology, becomes the Synthetic Methods of Glyoxalic Acid that domestic and international manufacturer generally adopts.
Glyoxal nitric acid oxidation method is under the catalytic action of the auxiliary agents such as hydrochloric acid, with nitric acid as oxidant selective oxidation glyoxal, generates principal product glyoxalic acid, and by-product oxalic acid.Reaction principle is as follows:
Main reaction equation is:
3CHO-CHO+2HNO
3→3CHO-COOH+2NO↑+H
2O①
Inevitably there is side reaction because glyoxalic acid is further oxided simultaneously, generate a certain amount of accessory substance oxalic acid.Side reaction equation is:
3CHO-COOH+2HNO
3→3HOOC-COOH+2NO↑+H
2O②
The synthetic method of current main flow also introduces air (containing the O of about 21%
2) participate in reaction, by the O in air
2nO is oxidized to NO
2, NO
2be only absorbed by the water reaction further, generate nitric acid or nitrous acid and become the oxidant of recoverable, solving problem of environmental pollution simultaneously.Mainly there is following reaction in this conversion process:
2NO+O
2＝2NO
2③
3NO
2+H
2O＝2HNO
3+NO④
4NO
2+O
2+2H
2O＝4HNO
3⑤
Investigate by literature search and to main manufacturer of the same trade, we find, have realized industrialized oxidation reaction apparatus and device for absorbing tail gas mainly contains following common feature existing and at present:
(1) oxidation furnaces is enamel stills for air blowing, and structure is too simple, can not meet the needs of oxidation reaction, can not
Adapt to the requirements such as optimization of process conditions well.
(2) tail gas absorption equipment adopts packed tower water to absorb mostly, and minority producer, with alkali liquor absorption device, reduces discharging with recovery oxidant nitric acid, but due to device level uneven, part producer the target of unrealized qualified discharge.
(3) common feature of oxidation furnaces and absorption equipment is, equipment is too simplified, unification, do not carry out appropriate design exploitation according to the characteristic of technique self and the principle of oxidation reaction and tail gas recycle improvement, generally adopt common apparatus but not special equipment.
Mainly there is following defect in above-mentioned existing apparatus:
Although A introduces air and participates in reaction, but this mainly introduces for NO being oxidized in tail gas absorption process NO2 reduction water absorption difficulty, the introducing of air does not have oxidizing reaction and itself causes much Beneficial Effects, do not make full use of the oxidant of overflowing from still from source to realize energy-saving and emission-reduction, thus tail gas generation is comparatively large, causes very large pressure to environmental protection.
B, mostly employing connect the equipment flowsheet of air-introduced machine at absorption tower end, reactor and absorption tower whole system are run under negative pressure, this can cause the rapid, high volume of sour gas in stills for air blowing to run off, and negative pressure is also unfavorable for that the water of gas absorbs, and makes desorb aggravate, makes the rate of recovery degradation of nitric acid, the concentration reclaiming nitric acid is also rarer, cause absorbing liquid total amount to strengthen, apply mechanically rear redundance and to have to treatment and discharge, be unfavorable for energy-saving and emission-reduction.
C, the oxidizing reaction temperature usually adopted are 50-80 DEG C, the gas temperature extracted out by negative pressure is up to 40-60 DEG C, cooling measure is not taked directly to enter absorption system, exothermic heat of reaction in simultaneously stability process, make to absorb temperature drift, absorb treatment effect not good, be unfavorable for improving raw materials recovery rate and reduction of discharging, and system cloud gray model is stable not, the phenomenon of discharge beyond standards happens occasionally.
Be 201420118230 in the patent No. to be called in the Chinese patent of " a kind of oxidation reaction of modified form synthesizing glyoxalic acid and the device of tail gas absorption ", be provided with tail gas condenser at the offgas outlet place of reactor, be convenient to comprise H by tail gas
2o, O
2, NO, NO
2hNO is formed by water vapor absorption
2and HNO
3again by being back in reactor after the brine ice cooling in tail gas condenser, reach and fully recycle tail gas, and maintain the stable of reactor internal oxidition environment, from source, directly fully recycle the oxidant of overflowing from reactor to realize energy-saving and emission-reduction.
But because from reactor, tail gas out enters into tail gas condenser, again to from the phegma after tail gas condenser cooling to this process of reactor, pipeline in coupled reaction still and tail gas condenser will be subject to violent variations in temperature, thus be very easy to be corroded aging, thus there is the problem of leaking.
Utility model content
For the deficiency that prior art exists, the purpose of this utility model is to provide a kind of oxidation reaction apparatus that can be good at the glyoxalic acid of pipeline between protective reaction still to tail gas condenser.
For achieving the above object, the utility model provides following technical scheme: a kind of oxidation reaction apparatus of glyoxalic acid, comprise reactor, tail gas condenser, absorption tower, absorbing liquid cooler, absorbing liquid circulating pump, described reactor comprises air inlet pipe and feed pipe, the offgas outlet place of described reactor is provided with tail gas condenser, described tail gas condenser is communicated with absorption tower, described absorption tower and described absorbing liquid cooler form cooling circuit by described absorbing liquid circulating pump, described device also comprises air blast, described air blast is connected with the air inlet pipe outer end of described reactor, described reactor is connected by return duct of giving vent to anger with tail gas condenser, described return duct of giving vent to anger also is provided with sealed tube outward, seal cavity is formed between the outer wall of described return duct of giving vent to anger and the inwall of sealed tube, the tube wall of described sealed tube is also connected with the air intake duct be communicated with seal cavity, the other end of air intake duct is connected with vavuum pump.
The utility model is set to further: one end tube head that described air inlet pipe and feed pipe stretch in reactor is closed, and the tube wall of described tube head is provided with multiple aperture.
The utility model is set to further: described absorption tower is the multistage ripple packing absorption tower of series connection, and described tower at different levels is respectively by described absorbing liquid circulating pump and the conducting of described absorbing liquid cooler.
The utility model is set to further: described tail gas condenser is shell and tube or enamel plate heat interchanger, and temperature-reducing medium is 0-15 DEG C of brine ice.
The utility model is set to further: described absorbing liquid cooler is the tubular heat exchanger of resistance to strong acid corrosion, the recirculated cooling water that temperature-reducing medium provides for cooling tower.
Compared with prior art, the utility model has the advantage of:
1, by adopting the brine ice in tail gas condenser to lower the temperature, make reactor gas phase escaping gas condensing reflux in reactor, the agent of abundant recycling partial oxidation also maintains the stable of still internal oxidition environment, fully recycles the oxidant of overflowing from still to realize energy-saving and emission-reduction from source.Achieve simultaneously tail gas enter absorption tower before precooling, be conducive to alleviating pipeline, equipment high temperature corrosion is aging, penetration enhancement process is normally carried out.
2, by being arranged on the sealed tube of giving vent to anger outside reflux line, then by air intake duct and vavuum pump, the seal cavity vacuum state that can will give vent to anger between return duct and sealed tube, when from reactor tail gas out and the condensate liquid that refluxes from tail gas condenser by give vent to anger return duct time, because it is outside in vacuum state, so avoid the risk of return duct of giving vent to anger from external corrosion, enhance its stability in use.
Accompanying drawing explanation
Fig. 1 is the system construction drawing of the oxidation reaction apparatus embodiment of a kind of glyoxalic acid of the utility model;
Fig. 2 is the sectional view of the return duct of giving vent to anger of the oxidation reaction apparatus embodiment of a kind of glyoxalic acid of the utility model, sealed tube and air intake duct.
In figure, 1, reactor; 2, air blast; 3, tail gas condenser; 4, absorption tower; 5, absorbing liquid circulating pump; 6, absorbing liquid cooler; 7, inlet valve; 8, intake valve; 9, air inlet pipe; 10, feed pipe; 11, agitator; 12, chuck; 13, steam valve; 14, cooling water valve; 15, outlet valve; 16, air outlet valve; 17, recovery valve; 18, valve is cooled; 19, absorption tower gas vent; 20, to give vent to anger return duct; 21, vavuum pump; 22, sealed tube; 221, seal cavity; 23, air intake duct; 24, mixed tail gas; 25, condensate liquid.
Detailed description of the invention
Be described further with reference to the oxidation reaction apparatus embodiment of Fig. 1 to a kind of glyoxalic acid of the utility model.
Air inlet pipe 9 is provided with in reactor 1, feed pipe 10 and agitator 11, air inlet pipe 9 and feed pipe 10 tube head stretched in reactor 1 are closed, the tube wall of tube head is provided with multiple aperture, by arranging multiple aperture at air inlet pipe pipeline section, air is made directly to enter liquid phase after aperture is uniformly distributed, realize NO fast to the conversion of NO2 and recycling, and avoid NO gas directly to escape from gas phase, make nitric acid in nitric acid dropping process be more evenly distributed simultaneously, alleviate the too high caused over oxidation of local concentration of nitric acid, decrease generation and other the side reaction of oxalic acid, improve principal product yield and product quality.The intake valve 8 for regulating air mass flow the outer end that air inlet pipe 9 stretches out reactor 1 is equipped with, the outer end that feed pipe 10 stretches out reactor 1 is provided with inlet valve 7, concrete, the air inlet pipe in the utility model embodiment and feed pipe are made up of the tubing of resistance to nitric acid and hcl corrosion.
Air inlet pipe 9 outer end connects medium-pressure or high pressure cfentrifugal blower 2, reactor and tail gas absorption whole system is made to become malleation from negative pressure, effectively reduce sour gas quick loss under negative pressure in reactor, add oxygen to recycle in the dissolving of liquid phase in the solubility of liquid phase and tail gas, and effectively inhibit the desorb in tail gas absorption process, improve the rate of recovery of nitric acid and reclaim the concentration (to 30-35%) of nitric acid, making the tail gas qualified discharge after process.The bottom of reactor 1 is provided with discharging opening, discharging opening is provided with outlet valve 15, after having reacted, open outlet valve 15, oxidation solution flows out the concentration kettle entering subsequent processing from discharging opening, the outer wall of reactor 1 is provided with the chuck 12 regulating temperature, chuck 12 is provided with Pressure gauge, steam inlet and coolant outlet, wherein, the position of steam inlet is higher than the position of coolant outlet, be convenient to the coolant outlet lower from position of the cooling water after steam liquefied discharge, steam inlet and coolant outlet are respectively equipped with steam valve 13 and cooling water valve 14, by steam regulation valve 13 and cooling water valve 14, control the temperature in chuck 12, make the reaction temperature in reactor 1 in the scope of process stipulation, reactor 1 is also provided with the common structure such as thermometer and Pressure gauge.
The top of reactor 1 is provided with gas outlet, gas outlet is provided with air outlet valve 16, the air inlet of tail gas condenser 3 is communicated with by conduit with the gas outlet of reactor 1, after reaction kettle for reaction completes, the tail gas produced in reactor 1 enters tail gas condenser 3 by gas outlet, H2O is comprised in mixed tail gas, O2, NO, NO2, in the utility model embodiment, tail gas condenser 3 is shell and tube or enamel plate heat interchanger, temperature-reducing medium is 0-15 DEG C of brine ice, the tail gas produced in reactor 1 forms HNO3 or HNO2 through water vapor absorption, brine ice cooling again in tail gas condenser 3, condensing reflux is in reactor 1, reach and fully recycle tail gas, and maintain the stable of reactor 1 internal oxidition environment, the oxidant directly fully recycling effusion from reactor 1 from source realizes energy-saving and emission-reduction.Achieve simultaneously tail gas enter absorption tower before precooling, be conducive to alleviating pipeline, equipment high temperature corrosion is aging, penetration enhancement process is normally carried out.
By being arranged on the sealed tube 22 of giving vent to anger outside return duct 20, then by air intake duct 23 and vavuum pump 21, seal cavity 221 vacuum state that can will give vent to anger between return duct 20 and sealed tube 22, when mixed tail gas 24 out and backflow from tail gas condenser 3 from reactor 1 condensate liquid 25 by give vent to anger return duct 20 time, because it is outside in vacuum state, so avoid the risk of return duct 20 of giving vent to anger from external corrosion, enhance its stability in use.
The tail gas that part is not reacted in tail gas condenser 3 enters absorption tower 4 by conduit, the outlet at bottom on absorption tower 4 is connected with absorbing liquid circulating pump 5, the other end of absorbing liquid circulating pump 5 connects the water inlet of absorbing liquid cooler 6 and the recovery port of Ethylene recov respectively, recovery valve 14 recovery port is equipped with, the delivery port of absorbing liquid cooler 6 is communicated with absorption tower 4, when closing recovery valve 14, absorption tower 4, absorbing liquid circulating pump 5 and absorbing liquid cooler 6 form cooling circuit, ceaselessly the liquid that completes in absorption tower 4 is sucked absorbing liquid cooler 6 by absorbing liquid circulating pump 5, be back in absorption tower 4 again, make water absorb this exothermic process to carry out at a lower temperature, improve the solubility of nitric acid and volatile gas, reduce desorb, absorb more abundant, facilitate the synchronous raising of the nitric acid rate of recovery and recovery concentration of nitric acid, particularly, in the utility model embodiment, absorbing liquid cooler is the tubular heat exchanger of resistance to strong acid corrosion, the recirculated cooling water that temperature-reducing medium provides for cooling tower, to be gone up to the air discharge by absorption tower gas vent 19.
The above is only preferred embodiment of the present utility model, protection domain of the present utility model be not only confined to above-described embodiment, and all technical schemes belonged under the utility model thinking all belong to protection domain of the present utility model.It should be pointed out that for those skilled in the art, do not departing from the some improvements and modifications under the utility model principle prerequisite, these improvements and modifications also should be considered as protection domain of the present utility model.
Claims (5)
1. the oxidation reaction apparatus of a glyoxalic acid, comprise reactor, tail gas condenser, absorption tower, absorbing liquid cooler, absorbing liquid circulating pump, described reactor comprises air inlet pipe and feed pipe, the offgas outlet place of described reactor is provided with tail gas condenser, described tail gas condenser is communicated with absorption tower, described absorption tower and described absorbing liquid cooler form cooling circuit by described absorbing liquid circulating pump, described device also comprises air blast, described air blast is connected with the air inlet pipe outer end of described reactor, it is characterized in that, described reactor is connected by return duct of giving vent to anger with tail gas condenser, described return duct of giving vent to anger also is provided with sealed tube outward, seal cavity is formed between the outer wall of described return duct of giving vent to anger and the inwall of sealed tube, the tube wall of described sealed tube is also connected with the air intake duct be communicated with seal cavity, the other end of air intake duct is connected with vavuum pump.
2. the oxidation reaction apparatus of a kind of glyoxalic acid according to claim 1, is characterized in that: one end tube head that described air inlet pipe and feed pipe stretch in reactor is closed, and the tube wall of described tube head is provided with multiple aperture.
3. the oxidation reaction apparatus of a kind of glyoxalic acid according to claim 2, is characterized in that: described absorption tower is the multistage ripple packing absorption tower of series connection, and described tower at different levels is respectively by described absorbing liquid circulating pump and the conducting of described absorbing liquid cooler.
4. the oxidation reaction apparatus of a kind of glyoxalic acid according to claim 1 or 2 or 3, is characterized in that: described tail gas condenser is shell and tube or enamel plate heat interchanger, and temperature-reducing medium is 0-15 DEG C of brine ice.
5. the oxidation reaction apparatus of a kind of glyoxalic acid according to claim 1, is characterized in that: described absorbing liquid cooler is the tubular heat exchanger of resistance to strong acid corrosion, the recirculated cooling water that temperature-reducing medium provides for cooling tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520778036.2U CN205032176U (en) | 2015-10-09 | 2015-10-09 | Oxidation reaction unit of glyoxalic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520778036.2U CN205032176U (en) | 2015-10-09 | 2015-10-09 | Oxidation reaction unit of glyoxalic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205032176U true CN205032176U (en) | 2016-02-17 |
Family
ID=55291111
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520778036.2U Expired - Fee Related CN205032176U (en) | 2015-10-09 | 2015-10-09 | Oxidation reaction unit of glyoxalic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN205032176U (en) |
-
2015
- 2015-10-09 CN CN201520778036.2U patent/CN205032176U/en not_active Expired - Fee Related
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160217 Termination date: 20171009 |