CN105289426A - Oxidation reaction device - Google Patents
Oxidation reaction device Download PDFInfo
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- CN105289426A CN105289426A CN201510789824.6A CN201510789824A CN105289426A CN 105289426 A CN105289426 A CN 105289426A CN 201510789824 A CN201510789824 A CN 201510789824A CN 105289426 A CN105289426 A CN 105289426A
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- hollow shaft
- kettle
- oxidation reaction
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Abstract
The invention discloses an oxidation reaction device, which comprises a self-suction type stirring reaction kettle, a condenser and an oxygen supply device, wherein the self-suction type stirring reaction kettle comprises a kettle body, an oxygen inlet chamber, a motor, a hollow shaft, a centrifugal impeller and a stirring impeller, the oxygen inlet chamber is hermetically fixed in the top of the kettle body, the upper end of the hollow shaft penetrates through the oxygen inlet chamber and is connected with the motor fixed on the kettle body, the centrifugal impeller is sleeved in the middle of the hollow shaft, the centrifugal impeller is provided with a feed hole and a discharge hole, and the feed hole is communicated with the oxygen inlet chamber through the hollow shaft; the stirring impeller is sleeved at the lower end of the hollow shaft; the oxygen supply device is communicated with an oxygen inlet chamber in the self-suction type stirring reaction kettle, and the top of the self-suction type stirring reaction kettle is provided with an air outlet communicated with a connecting pipe and a condenser; and a gas outlet of the condenser is communicated with the oxygen inlet chamber. The invention eliminates the discharge of waste gas, so that the reaction is rapid, the period is short, and the conversion rate and the yield of the product are high.
Description
Technical field
The present invention relates to technical field of chemical production equipment, especially a kind of oxidation reaction apparatus.
Background technology
In prior art, p-nitroacetophenone produces oxidation reaction apparatus, as shown in Figure 1, primarily of compositions such as oxidizing tower 1, air sparger 2, gas-liquid separator 3 and air compressors 5.After raw material nitro ethylbenzene adds oxidizing tower 1, the steam that tower body spacer passes into 0.6 ~ 0.8Mpa pressure carries out heat temperature raising to raw material, opens air compressor 5, the compressed air of commensurability 0.5 ~ 0.7Mpa pressure in tower when temperature is raised to about 130 ~ 140 DEG C.Compressed air is that rill enters in feed liquid by air sparger in tower 2 equiblibrium mass distribution.Because bubble proportion is much smaller than feed liquid; Therefore bubble floats naturally, again because bubble surface contacts in feed liquid, when reaching nitro ethylbenzene in oxygen reaction temperature, the oxygen in air rill just capable with raw material nitro ethylbenzene become oxidation reaction form p-nitroacetophenone.When air rill rises to raw material liquid level, other gas in rill and the complete oxygen of unreacted under the pressure of air compressor machine discharged to gas-liquid separator, the raw material of azeotropic under high temperature, high pressure and reaction of formation thing are separated backflow under the effect of separator in oxidizing tower 1, with the product in course of reaction and a large amount of tail gas discharged to after exhaust treatment system process again discharged to air; Air pollution must be caused like this, impact environment around.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, propose a kind of oxidation reaction apparatus, rational in infrastructure, pollution-free, energy consumption is low.
In order to realize foregoing invention object, the invention provides following technical scheme: a kind of oxidation reaction apparatus, comprise self-priming stirred autoclave, condenser and apparatus of oxygen supply, described self-priming stirred autoclave comprises kettle, enter oxygen room, motor, hollow shaft, centrifugal impeller and agitator arm, entering the sealing of oxygen room is fixed in kettle top, hollow shaft upper end is passed and is connected with the motor be fixed on kettle into oxygen room, described centrifugal impeller is set in the middle part of described hollow shaft, described centrifugal impeller is provided with charging hole and discharging opening, described charging hole through hollow shaft with enter oxygen room and be communicated with, described agitator arm is set in hollow shaft lower end, described apparatus of oxygen supply is communicated with the oxygen room of entering in described self-priming stirred autoclave, and described self-priming stirred autoclave top is provided with the gas outlet taken over and be communicated with condenser, the gas vent of described condensation channel with described enter oxygen room be communicated with.
Preferably, described apparatus of oxygen supply to be communicated with evaporimeter by liquid oxygen tank and to form, evaporator outlet with enter oxygen room and be communicated with.
Preferably, described evaporimeter and the passage entered between oxygen room are provided with flowmeter.
Preferably, also comprise water leg, described water leg is communicated with the liquid outlet of condensation channel.
Preferably, described kettle is jacket type structure.
Preferably, in described kettle, be provided with some attemperation of steam pipes, for heating the material in kettle.
Compared with prior art, the present invention has the following advantages: adopt sufficient pure oxygen directly to send into reactor, and guarantee that material reaction is complete, unnecessary oxygen, through condenser recycling use, eliminates the discharge of waste gas; And whole device is closed, and make to be swift in response, the cycle is short, conversion ratio and the yield of product are high.
Accompanying drawing explanation
Fig. 1 is the structural representation of traditional reaction unit;
Fig. 2 is the structural representation of oxidation reaction apparatus of the present invention.
Detailed description of the invention
Describe the present invention below in conjunction with accompanying drawing, the description of this part is only exemplary and explanatory, should not have any restriction to protection scope of the present invention.
A kind of p-nitroacetophenone as shown in Figure 2 produces oxidation reaction apparatus, comprise self-priming stirred autoclave 11, condenser 12, water leg 13 and apparatus of oxygen supply, self-priming stirred autoclave 11 comprises kettle, enter oxygen room 1-4, drive motors 1-1, hollow shaft 1-2, centrifugal impeller 1-6 and agitator arm 1-8, entering oxygen room 1-4 sealing is fixed in kettle top, hollow shaft 1-2 passes upper end and is connected with the drive motors 1-1 be fixed on kettle into oxygen room 1-4, centrifugal impeller 1-6 is set in the middle part of hollow shaft 1-2, centrifugal impeller 1-6 is provided with charging hole 1-7 and discharging opening, charging hole 1-7 through hollow shaft 1-2 with enter oxygen room 1-4 and be communicated with, agitator arm 1-8 is set in hollow shaft 1-2 lower end, apparatus of oxygen supply is communicated with the oxygen room 1-4 that enters in self-priming stirred autoclave 11, and self-priming stirred autoclave 11 top is provided with the gas outlet taken over and be communicated with condenser 12, the gas vent of condenser with enter oxygen room 1-4 and be communicated with, water leg 13 is communicated with the liquid outlet of condensation channel.
Apparatus of oxygen supply to be communicated with evaporimeter 14 by liquid oxygen tank 15 and to form, and evaporimeter 14 exports and enters oxygen room 1-4 and be communicated with, and evaporimeter 14 and the passage entered between the 1-4 of oxygen room are provided with flowmeter 16.
Kettle is jacket type structure; Some attemperation of steam pipe 1-5 are provided with, for heating the material in kettle in kettle.
After raw material nitro ethylbenzene joins self-priming stirred autoclave 11, the steam that temperature adjustment pipe 1-5 in still passes into about 0.6 ~ 0.8Mpa pressure is carried out heat temperature raising to raw material, when temperature is raised to about 130 ~ 140 DEG C, in still, enter from liquid oxygen tank 15, evaporimeter 14, flowmeter 16 etc. the high purity oxygen that oxygen room 1-4 passes into about 0.7 ~ 0.9Mpa pressure.The rotation of hollow shaft 1-2 is driven under the rotation of drive motors 1-1, again because centrifugal impeller 1-6 is contained on hollow shaft 1-2, so the synchronized rotation of centrifugal impeller 1-6 and hollow shaft 1-2, define raw material in still under the influence of centrifugal force to enter from centrifugal impeller charging hole 1-7, flow out from impeller discharging opening.Again owing to entering oxygen room 1-4 by oxygen uptake hole 1-3 on hollow shaft 1-2, hollow shaft 1-2 centre bore communicates with impeller charging hole 1-7, so rotate at centrifugal impeller, raw material makes oxygen uptake hole 1-3 define negative pressure relative to material in still when centrifugal impeller 1-6 high speed flows, oxygen suction is blended in feed liquid and forms fine gas bubbles, again under the effect of agitator arm 1-8 by gas, liquid is drop-down and fully stir, again because bubble surface contacts with feed liquid, when reaching nitro ethylbenzene and oxygen reaction temperature, oxygen in fine gas bubbles just generates nitro-acetophenone with raw material nitro oxidation reaction of ethylbenzene.
Because inside and outside for still gas circuit is designed to closed loop by this technique, when fine gas bubbles in feed liquid in still slowly rises to raw material liquid level, the vapour generated in the raw material of azeotropic and course of reaction under the oxygen that in fine gas bubbles, unreacted is complete and high temperature is entering the flows by action of negative relative in oxygen room 1-4 and still to condenser 12.When condenser 12 passes into cooling fluid, the raw material of the vapour and a small amount of azeotropic that react generation in gas can be separated and flow into water leg 13.The oxygen being separated after-purification through condenser 12 again due in self-priming stirred autoclave 11 with the effect of inlet plenum negative relative, the oxygen room of entering that self-priming turns back to self-priming stirred autoclave 11 participates in continuing reaction.
There is following advantage in reaction unit of the present invention:
1, closed loop pure oxygen reaction, eliminates the discharge of waste gas
Because this reaction unit have employed closed loop pure oxygen reaction environment, that enters still participation reaction does not just have other any gas.Not only because of the complete oxygen of previous unreacted after purification but also completely utilization and recycle, seldom the reaction gas compound of amount reclaims completely through condenser.So there is no gas and vapour discharge, completely solve a difficult problem for toxic emission and contaminated environment in gasification reaction.
The compressed air used at traditional type oxidation reaction apparatus, in air, usual oxygen content only has about 21%, the oxygen that can participate in reaction only has a few percent, reacted gas because of the decline of oxygen content cannot reuse, infiltrate in addition gas reactant because of large-minded recovery incomplete, so the environment that had a large amount of contaminated gas discharging to atmosphere pollution.
2, shorten the reaction time, improve the yield of product
Because this reaction unit have employed the reaction of closed loop pure oxygen, pure oxygen gas enters still and is blended into the fine gas bubbles surface participated in the nitro ethylbenzene liquid of reaction and is reactant.Transferring product to so react at a high speed when reaching reaction condition, shortening the reaction time, improve the conversion ratio of product and yield.
When homogeneity is with amount, conventional apparatus needs 24 hours, and this device only needs 18 hours.The conversion ratio of conventional apparatus is generally about 60%, and yield can only reach about 66%.The conversion ratio of this device is generally about 75%, and yield reaches about 80%.
3, circularly purifying, recovery oxygen are reused, and reclaim vapour and again utilize
This reaction unit is because adopting pure oxygen supply, when generating gasification byproducts in still internal cause course of reaction, when watering down oxygen suppression reaction, due to the active force of the special construction in still and centrifugal impeller, again because this technique gas circuit have employed the mode of closed cycle, air inlet and gas outlet in still is made to produce certain pressure reduction, gas reactor is flowed out outside still continuously, remove in course of reaction through condenser and generate gasification byproducts, oxygen after condensation cleaning, can reclaim closed cycle completely and flow back in still to go round and begin again and participate in reaction, until oxygen has consumed.The a small amount of raw material reclaimed through condensation, product, accessory substance utilize again.
In conventional apparatus, because tolerance is too large, heat energy is too high, cannot reclaim completely.
4, energy consumption has been saved
This reaction unit adopts pure supply without the need to pressurization, does not produce the power consumption of pressurization.Again due to pure oxygen reaction, outside flowing out still, throughput is minimum, so it is also little to take heat energy out of.
Tradition reaction unit, because using air, because oxygen content in air only has about 21%, must pressurize concentrated, improves oxygen density, improves oxidizing tower internal pressure.So a large amount of pressurization power consumptions will be consumed.When these a large amount of gases are in oxidizing tower, because the tower temperature in course of reaction is very high, absorb a large amount of heat energy again and take out of outside tower, from and consume a large amount of heating energy source.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. an oxidation reaction apparatus, it is characterized in that: comprise self-priming stirred autoclave, condenser and apparatus of oxygen supply, described self-priming stirred autoclave comprises kettle, enters oxygen room, motor, hollow shaft, centrifugal impeller and agitator arm, entering the sealing of oxygen room is fixed in kettle top, hollow shaft upper end is passed and is connected with the motor be fixed on kettle into oxygen room, described centrifugal impeller is set in the middle part of described hollow shaft, described centrifugal impeller is provided with charging hole and discharging opening, described charging hole through hollow shaft with enter oxygen room and be communicated with; Described agitator arm is set in hollow shaft lower end; Described apparatus of oxygen supply is communicated with the oxygen room of entering in described self-priming stirred autoclave, and described self-priming stirred autoclave top is provided with the gas outlet taken over and be communicated with condenser; The gas vent of described condenser with described enter oxygen room be communicated with.
2. oxidation reaction apparatus as claimed in claim 1, is characterized in that: described apparatus of oxygen supply to be communicated with evaporimeter by liquid oxygen tank and to form, evaporator outlet with enter oxygen room and be communicated with.
3. oxidation reaction apparatus as claimed in claim 2, is characterized in that: described evaporimeter and the passage entered between oxygen room are provided with flowmeter.
4. oxidation reaction apparatus as claimed in claim 1, it is characterized in that: also comprise water leg, described water leg is communicated with the liquid outlet of condensation channel.
5. oxidation reaction apparatus as claimed in claim 1, is characterized in that: described kettle is jacket type structure.
6. oxidation reaction apparatus as claimed in claim 1, is characterized in that: be provided with some attemperation of steam pipes in described kettle, for heating the material in kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510789824.6A CN105289426B (en) | 2015-11-17 | 2015-11-17 | Oxidation reaction device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510789824.6A CN105289426B (en) | 2015-11-17 | 2015-11-17 | Oxidation reaction device |
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| CN105289426A true CN105289426A (en) | 2016-02-03 |
| CN105289426B CN105289426B (en) | 2018-07-24 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202621181U (en) * | 2012-07-11 | 2012-12-26 | 宿迁科思化学有限公司 | Oxidization device |
| CN103657576A (en) * | 2013-11-27 | 2014-03-26 | 杭州海虹精细化工有限公司 | Apparatus for chlorine to oxidize ADC foaming agent tail gas |
| CN204159325U (en) * | 2014-08-21 | 2015-02-18 | 山东鲁化天九化工有限公司 | A kind of Novel mixer of the application in hydriding reactor |
| CN204503079U (en) * | 2015-03-05 | 2015-07-29 | 绵阳达高特新材料有限公司 | A kind of heterogeneous reaction agitator |
| CN204656501U (en) * | 2015-04-04 | 2015-09-23 | 中唯炼焦技术国家工程研究中心有限责任公司 | A kind of fixed-bed reactor efficiently preparing 9-Fluorenone |
| CN205164686U (en) * | 2015-11-17 | 2016-04-20 | 阜宁县安勤化学有限公司 | Oxidation reaction device |
-
2015
- 2015-11-17 CN CN201510789824.6A patent/CN105289426B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202621181U (en) * | 2012-07-11 | 2012-12-26 | 宿迁科思化学有限公司 | Oxidization device |
| CN103657576A (en) * | 2013-11-27 | 2014-03-26 | 杭州海虹精细化工有限公司 | Apparatus for chlorine to oxidize ADC foaming agent tail gas |
| CN204159325U (en) * | 2014-08-21 | 2015-02-18 | 山东鲁化天九化工有限公司 | A kind of Novel mixer of the application in hydriding reactor |
| CN204503079U (en) * | 2015-03-05 | 2015-07-29 | 绵阳达高特新材料有限公司 | A kind of heterogeneous reaction agitator |
| CN204656501U (en) * | 2015-04-04 | 2015-09-23 | 中唯炼焦技术国家工程研究中心有限责任公司 | A kind of fixed-bed reactor efficiently preparing 9-Fluorenone |
| CN205164686U (en) * | 2015-11-17 | 2016-04-20 | 阜宁县安勤化学有限公司 | Oxidation reaction device |
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| CN105289426B (en) | 2018-07-24 |
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Effective date of registration: 20220427 Address after: 224000 9 qinchuang Road, Qinnan Town, Yandu District, Yancheng City, Jiangsu Province Patentee after: Yancheng rijing Technology Co.,Ltd. Address before: 224403 No. 10, dinglan Road, Aoyang Industrial Park, Funing County, Yancheng City, Jiangsu Province Patentee before: FUNING COUNTY ANQIN CHEMICAL Co.,Ltd. |