CN205032174U - Do benefit to glyoxalic acid reaction unit of control raw materials input - Google Patents
Do benefit to glyoxalic acid reaction unit of control raw materials input Download PDFInfo
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- CN205032174U CN205032174U CN201520773735.8U CN201520773735U CN205032174U CN 205032174 U CN205032174 U CN 205032174U CN 201520773735 U CN201520773735 U CN 201520773735U CN 205032174 U CN205032174 U CN 205032174U
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- feed
- feeding
- input
- acid reaction
- glyoxalic acid
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Abstract
The utility model discloses a do benefit to glyoxalic acid reaction unit of control raw materials input, including reation kettle, tail gas condenser, absorption tower, absorption liquid cooler, absorption liquid circulating pump, reation kettle includes intake pipe and inlet pipe, the inlet pipe includes feeding house steward and at least one the feeding branch pipe that links to each other with it, a feeding intraductal feeding piston that is equipped with, be equipped with on the feeding piston and be used for material from the one -way feeding mechanism of feeding branch pipe to the circulation of feeding house steward orientation, the feeding branch pipe still is connected with the controlling means who is used for controlling feeding piston activity distance, through the activity distance of controlling means control feeding piston to control at every turn the feeding volume of feeding piston, be favorable to the input of controlled reaction raw materials, and then be favorable to the reaction to be spent completely.
Description
Technical field
The utility model relates to chemical reaction device field, in particular, relates to a kind of glyoxalic acid reaction device.
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;
D, cannot well control for the input quantity of raw material, usually the reacting dose of reactants occur glyoxal or nitric acid is not corresponding, thus causes the amount of glyoxal or nitric acid on the high side, and then has influence on last devil liquor recovery difficulty and become large.
Utility model content
For the deficiency that prior art exists, the glyoxalic acid reaction device that the purpose of this utility model is to provide a kind of reaction being conducive to ethylene glycol and nitric acid more complete.
For achieving the above object, the utility model provides following technical scheme: a kind of glyoxalic acid reaction device being beneficial to the input of control raw material, 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, at least one feed-inputing branched pipe that described feed pipe comprises charging house steward and is attached thereto, charging piston is provided with in described feed-inputing branched pipe, described charging piston is provided with the one-way feeding mechanism for being circulated from feed-inputing branched pipe to charging house steward direction by material, described feed-inputing branched pipe is also connected with the control device for controlling charging piston operating range.
The utility model is set to further: described control device comprises turning cylinder, described turning cylinder runs through to be located at feed-inputing branched pipe and to be controlled by motor, the part that described turning cylinder is arranged in feed-inputing branched pipe is provided with pars convoluta, be hinged with fork between described pars convoluta and charging piston, the axle center of turning cylinder is departed from the hinged place of described fork and pars convoluta.
The utility model is set to further: the sidewall of described feed-inputing branched pipe is provided with the installing hole for installing sealed bearing, and described turning cylinder matches with sealed bearing.
The utility model is set to further: described one-way feeding mechanism comprise run through charging piston run through through hole, described in run through through hole and be provided with jointed shaft near the side of charging house steward, described jointed shaft is hinged with for opening and closing the opening and closing element that this runs through through hole.
The utility model is set to further: described jointed shaft is provided with the torque spring making opening and closing element be tending towards running through described in closedown through hole trend.
The utility model is set to further: one end tube head that described air inlet pipe and charging house steward 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 provided with the control device of charging piston and control charging piston operating range on feed-inputing branched pipe, when control device drives charging piston back to move time, material can by the absorption of one-way feeding mechanism realization to material, when control device drive charging piston forward force feed time, material then can be transported to charging house steward by charging piston, be conducive to the control of the conveying capacity to material, when two feed-inputing branched pipes are set time, be conducive to the conveying of the inlet amount controlling ethylene glycol and nitric acid, make the reaction ratio of ethylene glycol and nitric acid more accurate, thus reaction is more complete, be conducive to the process of waste liquid.
Accompanying drawing explanation
Fig. 1 is the overall system structure schematic diagram of the present embodiment;
Fig. 2 is the structural representation of the inlet manifold of the present embodiment, air intake branch and control device;
Fig. 3 is the A portion enlarged drawing of Fig. 2;
Fig. 4 is the B portion enlarged drawing of Fig. 2;
Fig. 5 is the C portion enlarged drawing of Fig. 4.
In figure, 1, reactor; 2, air blast; 3, tail gas condenser; 4, absorption tower; 5, absorbing liquid circulating pump; 6, absorbing liquid cooler; 71, the first feed-inputing branched pipe; 72, the second feed-inputing branched pipe; 8, intake valve; 9, air inlet pipe; 10, charging house steward; 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, motor; 21, turning cylinder; 22, pars convoluta; 23, charging piston; 24, fork; 25, opening and closing element; 251, jointed shaft; 252, torque spring; 26, through hole is run through; 27, sealed bearing.
Detailed description of the invention
With reference to Fig. 1, a kind of glyoxalic acid reaction device embodiment controlling raw material input that is beneficial to of the utility model is described further.
Air inlet pipe 9, charging house steward 10 and agitator 11 is provided with in reactor 1, air inlet pipe 9 and charging house steward 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, make air directly enter liquid phase after aperture is uniformly distributed, realize NO fast to NO
2conversion 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 outer end that air inlet pipe 9 stretches out reactor 1 is equipped with the intake valve 8 for regulating air mass flow, the outer end that charging house steward 10 stretches out reactor 1 is provided with the first feed-inputing branched pipe 71 and the second feed-inputing branched pipe 72.
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, and 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, comprises H in mixed tail gas
2o, O
2, NO, NO
2, in the present embodiment, tail gas condenser 3 is shell and tube or enamel plate heat interchanger, and temperature-reducing medium is 0-15 DEG C of brine ice, and the tail gas produced in reactor 1 forms HNO through water vapor absorption
3or HNO
2brine ice cooling again in tail gas condenser 3, condensing reflux, in reactor 1, reaches and fully recycles tail gas, and maintaining 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.
With reference to Fig. 2 to Fig. 5, ethylene glycol can be led in the first feed-inputing branched pipe 71, logical nitric acid in the second feed-inputing branched pipe 72, by pre-setting the caliber of the first feed-inputing branched pipe 71 and the second feed-inputing branched pipe 72, and by fork 24 and pars convoluta 22 pin joint to turning cylinder 21 axis between deviation distance be set to unanimously, pressure in two arms is also set to unanimously, thus learns that the ratio of each inlet amount of ethylene glycol and nitric acid is exactly the ratio of the caliber of the first feed-inputing branched pipe 71 and the second feed-inputing branched pipe 72.
The rotation of turning cylinder 21 is driven by motor 20, also can drive the rotation of pars convoluta 22 simultaneously, thus fork 24 is by drive charging piston 23 moving back and forth in the first feed-inputing branched pipe 71 and the second feed-inputing branched pipe 72, simultaneously, at charging piston 23 toward when rollback, opening and closing element 25 will be backed down, ethylene glycol will be inhaled into the first feed-inputing branched pipe 71, nitric acid will be inhaled into the second feed-inputing branched pipe 72, when charging piston 23 forward impelling, closedown is run through through hole 26 by opening and closing element 25, ethylene glycol and nitric acid will be pressed into charging house steward 10 and then enter reactor 1, and close in order to still through hole 26 will be run through under better ensureing the state that opening and closing element 25 can be in stop motion at charging piston 23, described jointed shaft 251 is provided with the torque spring 252 making opening and closing element 25 be tending towards running through described in closedown through hole 26 trend.
Further, in order to ensure turning cylinder 21 and the connection sealing between the first feed-inputing branched pipe 71 and the second feed-inputing branched pipe 72 and rotate continuity, the sidewall of the first feed-inputing branched pipe 71 and the second feed-inputing branched pipe 72 is provided with the installing hole for installing sealed bearing 27, and described turning cylinder 21 matches with sealed bearing 27.
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 present 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 (9)
1. one kind is beneficial to the glyoxalic acid reaction device controlling raw material input, 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, at least one feed-inputing branched pipe that described feed pipe comprises charging house steward and is attached thereto, charging piston is provided with in described feed-inputing branched pipe, described charging piston is provided with the one-way feeding mechanism for being circulated from feed-inputing branched pipe to charging house steward direction by material, described feed-inputing branched pipe is also connected with the control device for controlling charging piston operating range.
2. a kind of glyoxalic acid reaction device being beneficial to the input of control raw material according to claim 1, it is characterized in that: described control device comprises turning cylinder, described turning cylinder runs through to be located at feed-inputing branched pipe and to be controlled by motor, the part that described turning cylinder is arranged in feed-inputing branched pipe is provided with pars convoluta, be hinged with fork between described pars convoluta and charging piston, the axle center of turning cylinder is departed from the hinged place of described fork and pars convoluta.
3. a kind of glyoxalic acid reaction device being beneficial to the input of control raw material according to claim 2, is characterized in that: the sidewall of described feed-inputing branched pipe is provided with the installing hole for installing sealed bearing, and described turning cylinder matches with sealed bearing.
4. a kind of glyoxalic acid reaction device being beneficial to the input of control raw material according to claim 1, it is characterized in that: described one-way feeding mechanism comprise run through charging piston run through through hole, the described through hole that runs through is provided with jointed shaft near the side of charging house steward, and described jointed shaft is hinged with for opening and closing the opening and closing element that this runs through through hole.
5. a kind of glyoxalic acid reaction device being beneficial to the input of control raw material according to claim 4, is characterized in that: described jointed shaft is provided with the torque spring making opening and closing element be tending towards running through described in closedown through hole trend.
6. a kind of glyoxalic acid reaction device being beneficial to the input of control raw material according to claim 1, it is characterized in that: one end tube head that described air inlet pipe and charging house steward stretch in reactor is closed, the tube wall of described tube head is provided with multiple aperture.
7. a kind of glyoxalic acid reaction device being beneficial to the input of control raw material according to claim 6, it 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.
8. a kind of glyoxalic acid reaction device being beneficial to the input of control raw material according to claim 1 or 6 or 7, it is characterized in that: described tail gas condenser is shell and tube or enamel plate heat interchanger, temperature-reducing medium is 0 ~ 15 DEG C of brine ice.
9. a kind of glyoxalic acid reaction device being beneficial to the input of control raw material 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 |
|---|---|---|---|
| CN201520773735.8U CN205032174U (en) | 2015-10-08 | 2015-10-08 | Do benefit to glyoxalic acid reaction unit of control raw materials input |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520773735.8U CN205032174U (en) | 2015-10-08 | 2015-10-08 | Do benefit to glyoxalic acid reaction unit of control raw materials input |
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| Publication Number | Publication Date |
|---|---|
| CN205032174U true CN205032174U (en) | 2016-02-17 |
Family
ID=55291109
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|---|---|---|---|
| CN201520773735.8U Expired - Fee Related CN205032174U (en) | 2015-10-08 | 2015-10-08 | Do benefit to glyoxalic acid reaction unit of control raw materials input |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116836493A (en) * | 2023-08-02 | 2023-10-03 | 山东华能线缆有限公司 | Polymer composite material for cables and preparation method thereof |
-
2015
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116836493A (en) * | 2023-08-02 | 2023-10-03 | 山东华能线缆有限公司 | Polymer composite material for cables and preparation method thereof |
| CN116836493B (en) * | 2023-08-02 | 2024-05-28 | 山东华能线缆有限公司 | Polymer composite material for cables and preparation method thereof |
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| 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 |
Granted publication date: 20160217 Termination date: 20171008 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |