CN205933230U - Collect device of nitrogen gas in follow cyclohexane oxidation tail gas - Google Patents

Collect device of nitrogen gas in follow cyclohexane oxidation tail gas Download PDF

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Publication number
CN205933230U
CN205933230U CN201620816152.3U CN201620816152U CN205933230U CN 205933230 U CN205933230 U CN 205933230U CN 201620816152 U CN201620816152 U CN 201620816152U CN 205933230 U CN205933230 U CN 205933230U
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gas
catalytic
temp
alternating temperature
oxidation
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陈恩之
姜曦
赵风轩
张银杏
万冬
陈东生
谯映辉
邓闯
高泉
张义全
谢毅
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Chengdu Plater Technology Co Ltd
Chongqing Huafeng Chemical Co Ltd
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Chengdu Plater Technology Co Ltd
Chongqing Huafeng Chemical Co Ltd
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Abstract

The utility model provides a collect device of nitrogen gas in follow cyclohexane oxidation tail gas, the device is including the alternating temperature adsorption equipment who is equipped with alternating temperature adsorbent layer who loops through the pipeline series connection, be equipped with the middle blender that meets air inlet that links to each other with compressed air source, heating device, catalytic oxidation device and the pressure swing adsorption device that is equipped with pressure swing adsorption agent layer, alternating temperature adsorption equipment adsorbs the dress ware including being equipped with the oxidation exhaust gas inlet and the alternating temperature absorption gas export alternating temperature that are linked together with the inner chamber, the catalytic oxidation device is including the catalytic oxidation ware that is equipped with the catalyst bed, catalytic oxidizer is equipped with the alternating temperature that is linked together rather than the inner chamber and adsorbs gas entry and the export of catalytic oxidation gas, the catalytic oxidation gas that is linked together with the inner chamber enters the mouth pressure swing adsorption unit and clean air out's pressure swing adsorption ware including being equipped with. The utility model discloses can obtain volume concentration and be the nitrogen gas more than 99.9%, not only retrieve the material, still reduce utility's consumption, reduce torch gas emission simultaneously.

Description

The device of nitrogen is collected from cyclohexane oxidation off-gas
Technical field
This utility model is related to the processing meanss of cyclohexane oxidation off-gas.
Background technology
Hexamethylene is a kind of important chemical intermediate, can oxidized generation cyclohexyl hydroperoxide, then decompose again Generate Hexalin and Ketohexamethylene.And Hexalin and Ketohexamethylene are all important industrial chemicals.And then produce caprolactam and nylon- 66.
At present, the no catalytic air oxidation method of hexamethylene is most popular method, instead of the oxygen deprivation oxidation of hexamethylene, Compared with oxygen deprivation oxidation, air oxidation process has the advantage that:
Required catalyst, the species of chemicals and quantity are few, and technological process is relatively easy, and equipment number of units significantly reduces, if Standby material requirement is low, and device gross investment is few, and operating pressure and temperature are low, and oxidation reactor and decomposition reactor are without special machine Process, longtime running not slagging scorification;The special alkali liquor piece-rate system of system configuration, enables device long-term operation, need not periodically stop Car is cleared up.
The waste liquid of the acid waste water produced by no catalytic air oxidation method of hexamethylene and catabolic process generation finally mixes Conjunction is delivered to salkali waste incinerator and is burned, and in the presence of auxiliary fuel, the calorific value by-product using the organic component in spent lye steams Vapour.The waste water negligible amounts of device discharge, oxidized tail gas then pass through extraction and absorb discharge torch.
But, there is oxidized tail gas amount greatly in current air oxidation of cyclohexane device, and directly discharge torch, causes resource Waste and serious environmental pollution, the wasting of resources.
Utility model content
Mesh of the present utility model is to disclose a kind of device collecting nitrogen from cyclohexane oxidation off-gas, to overcome existing skill The deficiency of art.
The device collecting nitrogen from cyclohexane oxidation off-gas described in the utility model, connects including passing sequentially through pipeline Connect is provided with the temperature swing absorption unit of temp.-changing adsorption oxidant layer, is provided with the centre connecing air intake being connected with compressed air source Blender, heater, catalytic oxidizing equipment and the pressure-swing absorption apparatus being provided with pressure-variable adsorption oxidant layer;
Described temperature swing absorption unit includes:
It is provided with the oxidized tail gas entrance with intracavity inter-connection and temp.-changing adsorption gas outlet temp.-changing adsorption dress device 102;
Described catalytic oxidizing equipment includes:
It is provided with the catalytic oxidizer of beds, described catalytic oxidizer is provided with the alternating temperature suction with its intracavity inter-connection Attached gas entrance and the outlet of catalysis oxidation gas;
Described pressure-swing absorption apparatus includes being provided with catalysis oxidation gas entrance with intracavity inter-connection and clean gas outlet Pressure swing adsorber;
Described pressure-variable adsorption agent is selected from molecular sieve or activated carbon;
Using device of the present utility model, the method collecting nitrogen from cyclohexane oxidation off-gas, comprise the steps:
(1) by the oxidized tail gas from air oxidation of cyclohexane device, send into temperature swing absorption unit, carry out temp.-changing adsorption, Operating condition is as follows:
Temperature be 15~30 DEG C of the oxidized tail gas time of staying in temperature swing absorption unit be 10~18 hours, pressure is 0.5~1.5MPa, temp.-changing adsorption agent is selected from activated carbon;
(2) the temp.-changing adsorption gas and compressed air of discharging temperature swing absorption unit are respectively fed to intermediate mixer mixing, become The weight ratio of warm adsorbed gas and compressed air is:
Temp.-changing adsorption gas: compressed air=6~10: 1, preferably 8: 1;
(3) intermediate mixer 4 mixed gas are sent into heater, be heated to 150~300 DEG C of temperature, then by top Enter catalytic reactor, the Organic substance in unstripped gas and oxygen occur oxidation reaction, generates carbon dioxide and water, and release a large amount of Reaction heat;Operating condition is as follows:
Temperature is 380~680 DEG C, preferably 630 DEG C, and air speed in catalytic reactor for the temp.-changing adsorption gas is 30~50h-1, Preferably 40h-1, pressure is 0.6~1MPa, preferably 0.8MPa;
Term " air speed " is defined as follows:The gas flow that in unit interval, per volume of catalyst is processed.
(4) subsequently into pressure-swing absorption apparatus, carry out pressure-variable adsorption, you can the volumetric concentration obtaining nitrogen is more than 99.9% Purification gas;
Operating condition is as follows:
Temperature is 40~50 DEG C, preferably 45 DEG C, and the time of staying in pressure-swing absorption apparatus 3 for the oxidized tail gas is 40~60 Second, preferably 50 seconds, pressure was 0.5~1.0MP.
The beneficial effects of the utility model are:Oxidized tail gas are not directly discharged to torch, first pass through temp.-changing adsorption, reclaim Organic substance in oxidized tail gas, more a small amount of Organic substance in tail gas is removed by catalytic oxidizing equipment 2, then pressure-swing absorption apparatus is pure Change, obtain the % nitrogen that volumetric concentration is more than 99.9.Not only reclaim material, also reduce the consumption of public work, simultaneously Reduce torch gas discharge capacity, there is significant Social and economic benef@.In terms of producing 80000000 Nm3 per year, capacity 8000 will be reduced Ten thousand Nm3, reduce 11,000,000 degree of the consumption of electricity.
Brief description
Fig. 1 is the schematic device collecting nitrogen from cyclohexane oxidation off-gas.
Fig. 2 is catalytic reactor structural representation.
Specific embodiment
Referring to Fig. 1 and Fig. 2, described in the utility model from cyclohexane oxidation off-gas collect nitrogen device, including according to Secondary it is provided with the temperature swing absorption unit 1 of temp.-changing adsorption oxidant layer 101, is provided with and is connected with compressed air source 6 by what pipeline was connected in series The intermediate mixer 4, heater 5, catalytic oxidizing equipment 2 and the change being provided with pressure-variable adsorption oxidant layer 301 that connect air intake 401 Pressure adsorbent equipment 3;
Described temperature swing absorption unit 1 includes:
It is provided with the oxidized tail gas entrance with intracavity inter-connection and the temp.-changing adsorption of temp.-changing adsorption gas outlet fills device 102;
Described catalytic oxidizing equipment 2 includes:
It is provided with the catalytic oxidizer 202 of beds 201, described catalytic oxidizer 202 is provided with and is connected with its inner chamber Logical temp.-changing adsorption gas entrance and the outlet of catalysis oxidation gas;
Preferably, described catalytic oxidizer 202, including upper catalytic bed 203 and lower catalytic bed 204, upper catalytic bed 203 He Catalytic oxidizer between lower catalytic bed 204 is provided with cold shock gas entrance 205, and described cold shock gas entrance 205 passes through pipeline and institute The mixed gas outlet of the intermediate mixer 4 stated is connected;
Preferably, it is provided between described upper catalytic bed 203 and lower catalytic bed 204 and described cold shock gas entrance 205 phase The gas distributor 206 of connection;
Described pressure-swing absorption apparatus 3 includes being provided with catalysis oxidation gas entrance with intracavity inter-connection and clean gas outlet Pressure swing adsorber 302;
Pressure-variable adsorption agent is selected from molecular sieve or activated carbon;
Preferably, also include torch, described torch passes through control valve and temp.-changing adsorption fills the oxidized tail gas entrance of device 102 It is connected;
The effect of torch is for cannot be carried out under process for producing device shutting down, improper production and the state of emergency effectively The fuel gas of recovery, flammable liquid.
Using device of the present utility model, the method collecting nitrogen from cyclohexane oxidation off-gas, comprise the steps:
(1) by the oxidized tail gas from air oxidation of cyclohexane device, send into temperature swing absorption unit 1, carry out temp.-changing adsorption, Operating condition is as follows:
Temperature be 15~30 DEG C of the oxidized tail gas time of staying in temperature swing absorption unit 1 be 10~18 hours, pressure For 0.5~1.5MPa;
Temp.-changing adsorption agent is selected from activated carbon;
(2) the temp.-changing adsorption gas and compressed air of discharging temperature swing absorption unit 1 are respectively fed to intermediate mixer 4 and mix, The weight ratio of temp.-changing adsorption gas and compressed air is:
Temp.-changing adsorption gas: compressed air=6~10: 1, preferably 8: 1;
(3) intermediate mixer 4 mixed gas are sent into heater 5, be heated to 150~300 DEG C of temperature, then by top Enter catalytic reactor, the Organic substance in unstripped gas and oxygen occur oxidation reaction, generates carbon dioxide and water, and release a large amount of Reaction heat;Operating condition is as follows:
Temperature is 380~680 DEG C, preferably 630 DEG C, and air speed in catalytic reactor for the temp.-changing adsorption gas is 30~50h-1, Preferably 40h-1, pressure is 0.6~1MPa, preferably 0.8MPa;
Term " air speed " is defined as follows:The gas flow that in unit interval, per volume of catalyst is processed.
Preferably, the mixed gas of intermediate mixer 4, are partially into heater 5, are heated to 150~300 DEG C of temperature, Then catalytic reactor is entered by top;
The mixed gas of the intermediate mixer 4 of surplus pass through the cold shock gas entrance 205 of catalytic oxidizer, enter catalysis oxidation Device, mixes intensification by gas distributor with the reaction gas getting off in top, enters reactor second layer beds and carries out instead Should;
The mixed gas of the intermediate mixer 4 of surplus are the 45~50% of the mixed gas cumulative volume of intermediate mixer 4;
The operating condition of ground floor beds is as follows:
Temperature is 580~680 DEG C, preferably 630 DEG C, and air speed in catalytic reactor for the temp.-changing adsorption gas is 30~50h-1, Preferably 40h-1, pressure is 0.6~1MPa, preferably 0.8MPa;
The operating condition of second layer beds is as follows:
Temperature is 530~630 DEG C, preferably 580 DEG C, and air speed in catalytic reactor for the temp.-changing adsorption gas is
30~50h-1, preferably 40h-1, pressure is 0.6~1MPa, preferably 0.8MPa;
Catalyst is de- hydrocarbon catalyst, has low form and high temperature modification, is mixed packing;
(4) subsequently into pressure-swing absorption apparatus 3, carry out pressure-variable adsorption, you can the volumetric concentration obtaining nitrogen is more than 99.9% purification gas;
Operating condition is as follows:
Temperature is 40~50 DEG C, preferably 45 DEG C, and the time of staying in pressure-swing absorption apparatus 3 for the oxidized tail gas is 40~60 Second, preferably 50 seconds, pressure was 0.5~1.0MP;Pressure-variable adsorption agent is selected from molecular sieve or activated carbon.
Embodiment 1
Using the flow process of Fig. 1 and the reactor of Fig. 2.
Basic parameter:
In the oxidized tail gas of air oxidation of cyclohexane device, the volumetric concentration 96.4% of nitrogen;
Temp.-changing adsorption agent is activated carbon;
Catalyst is de- hydrocarbon catalyst, has low form and high temperature modification, is mixed packing;
Pressure-variable adsorption agent is activated carbon.
(1) temp.-changing adsorption, operating condition is as follows:
Temperature is 25 DEG C, and the time of staying in temperature swing absorption unit 1 for the oxidized tail gas is 14 hours, and pressure is 0.9MPa;
(2) the weight ratio of temp.-changing adsorption gas and compressed air is:Temp.-changing adsorption gas: compressed air=8:1;
(3) mixed gas of intermediate mixer 4, are partially into heater 5, are heated to 230 DEG C of temperature, then by top Enter catalytic reactor;
The mixed gas of the intermediate mixer 4 of surplus pass through the cold shock gas entrance 205 of catalytic oxidizer, enter catalysis oxidation Device;
The mixed gas of the intermediate mixer 4 of surplus are the 50% of the mixed gas cumulative volume of intermediate mixer 4;
The operating condition of ground floor beds is as follows:
Temperature is 630 DEG C, and air speed in catalytic reactor for the temp.-changing adsorption gas is 40h-1, pressure is 0.8MPa;
The operating condition of second layer beds is as follows:
Temperature is 580 DEG C, and air speed in catalytic reactor for the temp.-changing adsorption gas is 40h-1, pressure is 0.8MPa;
(4) operating condition of pressure-swing absorption apparatus 3 is as follows:
Temperature is 45 DEG C, and the time of staying in pressure-swing absorption apparatus 3 for the oxidized tail gas is 50 seconds, and pressure is 0.75MPa;
In the purification gas obtaining, the volumetric concentration of nitrogen is 99.99%.
Embodiment 2
Using the flow process of Fig. 1 and the reactor of Fig. 2
Basic parameter:
In the oxidized tail gas of air oxidation of cyclohexane device, the volumetric concentration 96.4% of nitrogen;
Temp.-changing adsorption agent is activated carbon;
Catalyst is de- hydrocarbon catalyst, has low form and high temperature modification, is mixed packing;
Pressure-variable adsorption agent is molecular sieve.
(1) temp.-changing adsorption, operating condition is as follows:
Temperature is 30 DEG C, and the time of staying in temperature swing absorption unit 1 for the oxidized tail gas is 16 hours, and pressure is 1MPa;
(2) the weight ratio of temp.-changing adsorption gas and compressed air is:Temp.-changing adsorption gas: compressed air=10:1;
(3) mixed gas of intermediate mixer 4, are partially into heater 5, are heated to 210 DEG C of temperature, then by top Enter catalytic reactor;
The mixed gas of the intermediate mixer 4 of surplus pass through the cold shock gas entrance 205 of catalytic oxidizer, enter catalysis oxidation Device;
The mixed gas of the intermediate mixer 4 of surplus are the 45% of the mixed gas cumulative volume of intermediate mixer 4;
The operating condition of ground floor beds is as follows:
Temperature is 630 DEG C, and air speed in catalytic reactor for the temp.-changing adsorption gas is 35h-1, pressure is 0.8MPa;
The operating condition of second layer beds is as follows:
Temperature is 580 DEG C, and air speed in catalytic reactor for the temp.-changing adsorption gas is 35h-1, pressure is 0.8MPa;
(4) operating condition of pressure-swing absorption apparatus 3 is as follows:
Temperature is 40 DEG C, and the time of staying in pressure-swing absorption apparatus 3 for the oxidized tail gas is 45 seconds, and pressure is 0.75MPa;
In the purification gas obtaining, the volumetric concentration of nitrogen is 99.99%.

Claims (4)

1. collect the device of nitrogen from cyclohexane oxidation off-gas it is characterised in that including passing sequentially through what pipeline was connected in series It is provided with the temperature swing absorption unit (1) of temp.-changing adsorption oxidant layer (101), be provided with and connect air intake with compressed air source (6) is connected (401) intermediate mixer (4), heater (5), catalytic oxidizing equipment (2) and the transformation being provided with pressure-variable adsorption oxidant layer (301) Adsorbent equipment (3);
Described temperature swing absorption unit includes being provided with oxidized tail gas entrance and temp.-changing adsorption gas outlet alternating temperature with intracavity inter-connection Absorption dress device (102);
Described catalytic oxidizing equipment (2) includes:
It is provided with the catalytic oxidizer (202) of beds, described catalytic oxidizer is provided with the alternating temperature with its intracavity inter-connection Adsorbed gas entrance and the outlet of catalysis oxidation gas;
Described pressure-swing absorption apparatus includes being provided with and the catalysis oxidation gas entrance of intracavity inter-connection and the transformation of clean gas outlet Adsorber (302).
2. device according to claim 1 it is characterised in that described catalytic oxidizer include catalytic bed (203) and Lower catalytic bed (204), the catalytic oxidizer between upper catalytic bed (203) and lower catalytic bed (204) is provided with cold shock gas entrance (205), described cold shock gas entrance (205) is connected with the mixed gas outlet of described intermediate mixer (4) by pipeline.
3. device according to claim 2 it is characterised in that described upper catalytic bed (203) and lower catalytic bed (204) it Between be provided with the gas distributor (206) being connected with described cold shock gas entrance (205).
4. it is characterised in that also including torch, described torch passes through control to the device according to any one of claims 1 to 3 The oxidized tail gas entrance that valve processed fills device with temp.-changing adsorption is connected.
CN201620816152.3U 2016-07-28 2016-07-28 Collect device of nitrogen gas in follow cyclohexane oxidation tail gas Active CN205933230U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106082145A (en) * 2016-07-28 2016-11-09 重庆华峰化工有限公司 The apparatus and method of nitrogen are collected from cyclohexane oxidation off-gas

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106082145A (en) * 2016-07-28 2016-11-09 重庆华峰化工有限公司 The apparatus and method of nitrogen are collected from cyclohexane oxidation off-gas
CN106082145B (en) * 2016-07-28 2018-07-10 重庆华峰化工有限公司 The device and method that nitrogen is collected from cyclohexane oxidation off-gas

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