CN209952482U - Device for purifying yellow phosphorus tail gas - Google Patents
Device for purifying yellow phosphorus tail gas Download PDFInfo
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- CN209952482U CN209952482U CN201920429219.1U CN201920429219U CN209952482U CN 209952482 U CN209952482 U CN 209952482U CN 201920429219 U CN201920429219 U CN 201920429219U CN 209952482 U CN209952482 U CN 209952482U
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Abstract
The utility model discloses a purify device of yellow phosphorus tail gas, including the scrubbing tower, desulfurizing tower, fixed bed and the adsorption component who connects gradually, establish yellow phosphorus tail gas import on the scrubbing tower, pack the dephosphorization adsorbent in the fixed bed, adsorption component includes the temperature swing adsorption bed, establishes the export of just purifying gas on the temperature swing adsorption bed. The utility model discloses a scrubbing tower, desulfurizing tower, fixed bed and the absorption subassembly that connects gradually form, and yellow phosphorus tail gas obtains just purifying gas after washing, desulfurization, dephosphorization, alternating temperature absorption, not only can be used to the boiler and produce steam, generate electricity and to the industrial device that CO impurity requirement is not high, has more solved prior art device working costs height, and the operation is unstable and waste water discharge is big etc. shortcoming.
Description
Technical Field
The utility model belongs to the technical field of gaseous purification, specific purify device of yellow phosphorus tail gas that says so.
Background
According to incomplete statistics, the production scale of yellow phosphorus is more than 60 million tons in 2015, each 1 ton of yellow phosphorus is produced and a byproduct of 2500 ~ cubic meters of tail gas contains 85 ~% of CO, and also contains a large amount of toxic substances such as fluorine, phosphorus, sulfur, arsenic and the like and raw material dust, and the like.
The existing yellow phosphorus tail gas treatment methods comprise a water washing method, a water washing and alkali washing method, a sodium hypochlorite method, an activated carbon fixed bed catalytic oxidation method, a PDS desulfurization and temperature swing adsorption method and the like, and have the following defects:
A. a water washing method: the purification precision is poor, and the method is only suitable for the primary utilization of the yellow phosphorus tail gas.
B. Water washing and alkali washing: large alkali liquor consumption, large sewage treatment capacity, organic sulfur and PH3Difficult to remove.
C. Sodium hypochlorite method: can oxidize a large amount of H2S、PH3And a small amount of organic sulfur needs to be washed with alkali to remove fluorine, but the sewage quantity is large, and the organic sulfur is difficult to remove.
D. The activated carbon fixed bed catalytic oxidation method: the dephosphorization effect is good, but a large amount of activated carbon is consumed, the activated carbon has strong adsorbability to phosphorus compounds and is difficult to regenerate, and the activated carbon is subject to the fluctuation of phosphorus and sulfur in tail gas, so that the activated carbon is quick to lose efficacy.
E. PDS desulfurization and temperature swing adsorption method: PDS desulfurization can remove most of inorganic sulfur, HF and part of organic sulfur, temperature swing adsorption can remove the remaining sulfide, phosphorus, arsenic, fluorine and the like, the method is to remove phosphorus elementary substance solid with high boiling point and PH3 gas with low boiling point together, the boiling point of the phosphorus elementary substance P4 is 280 ℃, the boiling point of phosphine is-87.7 ℃, low-pressure superheated steam with the temperature of more than 400 ℃ is usually adopted for regeneration of an adsorbent, and the steam consumption is greatly increased along with the increase of the content of phosphorus and sulfur in tail gas, so that the defect of high operation cost of the device is caused.
To better realize the PH value of the yellow phosphorus tail gas3For removal of (B), the prior patent document CN101564637 (PH in tail gas of yellow phosphorus furnace)32009.10.28) discloses a method for removing yellow phosphorus from the tail gas of a yellow phosphorus furnace, introducing the tail gas into a dust-removing phosphorus-removing tank to remove elemental yellow phosphorus and phosphorus pentoxide, then sending the tail gas into an alkali absorption tower to remove acid gas by using a desulfurizing agent, sending the tail gas into a dephosphorization tower, and spraying and absorbing PH by using potassium permanganate solution3The method of (1). Can effectively remove SO in the yellow phosphorus tail gas2、HF、PH3、AsH3And the like.
In addition, patent document CN1345619A (method for removing phosphorus, phosphide, and sulfide from yellow phosphorus tail gas, 2002.04.24) discloses a gas separation method for obtaining purified gas by removing acidic components from yellow phosphorus tail gas through an alkaline washing process, removing phosphorus from the tail gas through a pretreatment process using a carbonaceous adsorbent, and adsorbing and removing phosphide and sulfide through an adsorbent in a pressure swing temperature adsorption process. Simple operation, the content of phosphorus and other compounds in the purified gas is less than 1ppm, and the content of sulfur compounds is less than 1 ppm. In the prior art, patent document CN106085530 (a process for co-producing liquefied natural gas and food grade carbon dioxide by using yellow phosphorus tail gas, 2016.06.21) discloses a process for preparing liquefied natural gas and food grade carbon dioxide by purifying yellow phosphorus tail gas through steps of water washing, compression, PDS wet desulphurization, temperature swing adsorption, sulfur-tolerant isothermal transformation, deep purification, methanation, decarburization, cryogenic liquefaction and the like, which can effectively realize zero carbon emission.
The yellow phosphorus tail gas purification method described in the above patent document does not completely solve the drawbacks of the prior art, and therefore the present invention is suitable for transportation.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a purify device of yellow phosphorus tail gas, the scrubbing tower, desulfurizing tower, fixed bed and the absorption subassembly that adopt to connect gradually are constituteed, and yellow phosphorus tail gas obtains just purifying gas after washing, desulfurization, dephosphorization, alternating temperature absorption, not only can be used to the boiler and produces steam, generate electricity and to the industrial device that CO impurity requirement is not high, has more solved prior art device working costs height, and the operation is unstable and shortcoming such as waste water discharge is big.
The utility model discloses a following technical scheme realizes: the utility model provides a purify device of yellow phosphorus tail gas, includes scrubbing tower, desulfurizing tower, fixed bed and the adsorption component who connects gradually, establishes yellow phosphorus tail gas import on the scrubbing tower, packs the dephosphorization adsorbent in the fixed bed, and the adsorption component includes the temperature swing adsorption bed, establishes the gas outlet that just purifies on the temperature swing adsorption bed.
In the utility model, the washing tower adopts the circulating spray water to roughly wash the yellow phosphorus tail gas from the phosphorus furnace, and the dust and part of element phosphorus in the yellow phosphorus tail gas are removed through full contact of gas and liquid; the desulfurization tower adopts wet desulfurization to remove the hydrogen sulfide in the yellow phosphorus tail gas to 20mg/Nm3The organic sulfur is removed by 40 ~ 80%, and hydrogen fluoride is removed at the same time, zeolite, active carbon and the like are adopted as dephosphorizing absorbent in the fixed bed for removing simple substance P in yellow phosphorus tail gas4(ii) a The temperature swing adsorption bed can adjust the PH value remained in the tail gas3、AsH3Sulfur and other low boilingThe point impurity is removed to below 1ppm and is sent out from the outlet of the primary purified gas, and the primary purified gas can be used for steam production of boilers, power generation and industrial devices with low requirements on CO impurities.
The utility model also comprises a fine desulfurizing tower, a fine desulfurizing and dearsenifying tower and a fine defluorinating tower which are connected in sequence, wherein the primary purified gas outlet is connected with the fine desulfurizing tower, the fine defluorinating tower is provided with a fine purified gas outlet which can deeply purify the primary purified gas to remove the sulfur, the phosphorus, the arsenic and the fluorine below 0.1ppm to obtain the fine purified gas, and the fine purified gas can be used for producing various chemical products such as natural gas, methanol, dimethyl ether, acetic acid, glycol and the like,
the adsorption component also comprises a pressure swing adsorption tower group, the pressure swing adsorption tower group is composed of two stages of pressure swing adsorption towers which are connected in series, the primary purified gas outlet is connected with the pressure swing adsorption tower which is positioned at the first stage, the fine purified gas outlet is arranged on the pressure swing adsorption tower which is positioned at the last stage, and the two stages of pressure swing adsorption towers are arranged, and the CO can be removed by the one stage of pressure swing adsorption tower2And other impurities, the secondary pressure swing adsorption tower can be used for purifying CO, and the requirement on the purity of the raw materials of the carbon chemical products is met.
The fixed bed is internally provided with a steam regeneration system for regenerating the dephosphorizing adsorbent, the fixed bed is provided with a steam inlet and a steam outlet which are communicated with the steam regeneration system, the dephosphorizing adsorbent is regenerated by superheated steam after being saturated in adsorption, the regenerated dephosphorizing adsorbent can be adsorbed again, and when the dephosphorizing adsorbent loses efficacy, the dephosphorizing adsorbent can be sent to a phosphorus furnace for recycling, and a large amount of phosphorus simple substances can be recovered.
The number of the temperature swing adsorption beds is at least 5, at least two adsorbents are filled in each temperature swing adsorption bed, when the temperature swing adsorption bed is used, the 5 temperature swing adsorption beds are continuously recycled, and a cyclic adsorption process is completed after adsorption, pressure reduction, hot blowing, cold blowing and pressure increase are respectively carried out.
And a pressurizing device, such as a water ring pump, is arranged between the washing tower and the desulfurizing tower, and can pressurize the washed yellow phosphorus tail gas to 20 ~ 200kPa for wet desulfurization.
Compared with the prior art, the utility model, following advantage and beneficial effect have:
(1) existing yellow phosphorus purifying toolThe temperature swing adsorption involved in the process generally considers the phosphorus simple substance P with high boiling point4Solids and low boiling point pH3Removal of gas together, pH3Easily penetrate the bed layer and phosphorus simple substance P4The boiling point of (A) is 280 ℃, so that the bed layer is usually regenerated by using low-pressure superheated steam with the temperature of above 400 ℃, so that a large amount of steam is consumed, and the running cost of the device is high. Therefore, the utility model adopts the fixed bed and the temperature swing adsorption bed which are connected in sequence to respectively treat P with high boiling point4Equal solid impurities and low boiling point PH3Removing the residual PH in the tail gas by adopting a temperature swing adsorption bed on one hand3、AsH3Sulfur and other low-melting-point impurities, the regeneration gas can be steam, nitrogen and crude purified gas with the temperature of 100 ~ 200 ℃ to reduce the steam consumption and save the energy consumption, and on the other hand, the dephosphorizing adsorbent of the fixed bed is adopted to remove the elemental phosphorus P firstly4And other high boiling point impurities, the adsorbent has long service life, and can be replaced for half a year, a year or longer, so that the operation cost is greatly reduced.
(2) The utility model discloses in, the fixed bed can adopt zeolite, active carbon etc. as dephosphorizing adsorbent, and during the specific use, the active carbon of adsorption saturation blows off absorbent PH3Then the mixture is sent into a phosphorus furnace for recycling, and the adsorbed phosphorus simple substance P can be recycled4Recovering; the dephosphorizing adsorbent can also be regenerated by utilizing superheated steam, and the dephosphorizing adsorbent is sent to a phosphorus furnace for recycling after being out of service.
(3) The invention solves the defects of high running cost, unstable operation, incomplete impurity removal, difficult adsorbent regeneration, large wastewater discharge and the like of the device in the prior art, and the gas subjected to temperature swing adsorption is primary purified gas and can be used for industrial devices which have low requirements on steam generation, power generation and CO impurities of boilers; the purified gas after deep purification can be used for producing various carbon chemical products, such as natural gas, methanol, dimethyl ether, acetic acid, ethylene glycol and the like.
Drawings
Fig. 1 is a schematic view (a) of the process flow of the present invention.
Fig. 2 is a schematic view of the process flow of the present invention (ii).
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited thereto.
Example 1:
this embodiment provides a device for purifying yellow phosphorus tail gas.
As shown in fig. 1, the device comprises a washing tower, a pressurizing device, a desulfurizing tower, a fixed bed, an adsorption component and a deep purification unit which are connected in sequence, wherein a yellow phosphorus tail gas inlet is arranged on the washing tower; the fixed bed is filled with a dephosphorizing adsorbent, a steam regeneration system for regenerating the dephosphorizing adsorbent is arranged in the fixed bed, and a steam inlet and a steam outlet which are communicated with the steam regeneration system are arranged on the fixed bed; the adsorption component comprises a temperature swing adsorption bed, and a primary purified gas outlet is arranged on the temperature swing adsorption bed; the deep purification unit comprises a fine desulfurization tower, a fine desulfurization dearsenification tower and a fine defluorination tower which are connected in sequence, wherein a primary purified gas outlet is connected with the fine desulfurization tower, and a fine purified gas outlet is arranged on the fine defluorination tower.
The specific process flow of this example is as follows:
(1) washing with water: 20000Nm from phosphorus furnace3And h, sending the yellow phosphorus tail gas into a washing tower from a yellow phosphorus tail gas inlet, roughly washing the yellow phosphorus tail gas in the washing tower through circulating spray water, and removing dust and part of element phosphorus in the tail gas through full contact of gas and liquid.
(2) Pressurizing: pressurizing the yellow phosphorus tail gas after water washing to 20kPa by a water ring pump.
(3) And (3) wet desulphurization: the hydrogen sulfide in the pressurized yellow phosphorus tail gas is removed to 20mg/Nm by adopting a desulfurizing tower3The organic sulfur is removed by 40 ~ 80%, and hydrogen fluoride is removed at the same time, the alkaline solution (such as ammonia water or alkaline solution) containing binuclear cobalt phthalocyanine sulfonate is used as an absorbent in the desulfurizing tower, belonging to a liquid phase catalytic oxidation method.
(4) Dephosphorizing elemental P4: treating the tail gas after wet desulphurization by using a fixed bed filled with dephosphorizing adsorbents such as zeolite and active carbon to remove high-boiling-point simple substance P in the yellow phosphorus tail gas4And other high boiling point impurities, such as tar, naphthalene, arsenic, etc. through the process, P in the yellow phosphorus tail gas4Is removed fromWhen the pH value is more than 90 percent, the adsorbed pH value is blown off by the activated carbon with saturated adsorption3Then the mixture is sent into a phosphorus furnace for recycling, and the adsorbed phosphorus simple substance P can be recycled4And (6) recovering.
(5) Temperature swing adsorption:
a temperature swing adsorption system consisting of five towers is adopted, adsorbents such as active carbon and the like are filled in a temperature swing adsorption bed, and the regeneration gas adopts saturated steam with the temperature of 140 ℃. Can remove residual PH in the tail gas3、AsH3Sulfur and other low-melting point impurities are removed to below 1 ppm. The gas at the outlet is the primary purified gas which can be used for industrial devices with low requirements on steam generation, power generation and CO impurities of boilers. In this embodiment, the temperature swing adsorption beds are all composite beds, at least two different adsorbents are filled in the same adsorption bed, the adsorption beds in the impurity removal system constitute a continuous operation system, and each adsorption bed undergoes the following processes in one cycle period:
adsorption (a): and (3) enabling the desulfurized purified gas to enter from the bottom of the TSA adsorber, and enabling impurity components such as phosphorus, arsenic, sulfur and the like in the gas to be adsorbed by the adsorbent in the adsorption bed to obtain the purified yellow phosphorus tail gas. When the adsorption bed reaches saturated adsorption, the adsorption is stopped. The purified yellow phosphorus tail gas enters a product gas buffer tank and then is treated by a sulfur-tolerant shift process;
pressure reduction (B): after the adsorption step is finished, opening a pressure reduction valve, and automatically removing gas in the adsorption bed from the bottom of the adsorption bed by depending on the pressure in the adsorption bed;
hot blowing (H), wherein the regenerated gas can use steam, nitrogen and crude purified gas with the temperature of 100 ℃ of ~ 200 ℃ for heating the adsorption bed, the regenerated gas enters the adsorption bed from the top of the TSA adsorber, the temperature of the adsorption bed is raised, so that adsorbed impurities are vaporized and are taken out from the bottom of the adsorption bed along with the regenerated gas, so that an adsorbent is regenerated, mixed gas discharged from the bottom enters a spray tower, after being sprayed with cooling water, the gas enters a waste gas-water separator for separation, the obtained non-condensable gas is sent to a torch or a phosphorus furnace, waste liquid is sent to a waste water tank, liquid obtained after spraying is treated by a phosphorus mud filter, and the obtained phosphorus mud is sent to a phosphorus mud tank;
cold blowing (C): and (4) opening a cold blowing valve, performing cold blowing on part of the purified yellow phosphorus tail gas, entering from the top of the TSA adsorber, and taking out the waste heat in the adsorption bed until the bed temperature reaches the air inlet temperature during adsorption. And cooling the cold blowing gas discharged from the bottom of the TSA adsorber by a cold blowing gas cooler, and then separating the cold blowing gas in a cold blowing gas-water separator. The gas obtained by separation enters a TSA purified gas buffer tank and enters the subsequent working procedure together with the purified yellow phosphorus tail gas; the waste liquid obtained by separation is sent to a waste water tank;
pressure increase (R): and (4) slowly pressurizing the adsorption bed by using the purified yellow phosphorus tail gas until the normal adsorption working pressure is reached, and waiting for the next adsorption process.
(6) Deep purification: pressurizing the primary purified gas to 1.0MPa, and sequentially passing through a fine desulfurization tower, a fine desulfurization dearsenification tower and a fine defluorination tower to remove phosphorus, sulfur, arsenic and fluorine in the primary purified gas to be below 0.1ppm to obtain the fine purified gas, wherein the fine purified gas can be used for metallurgical devices with higher requirements on the content of phosphorus, sulfur, arsenic and fluorine impurities.
In the deep purification process, hydrolysis desulfurization and CS are adopted for desulfurization2COS is a relatively common organic sulfur form and is difficult to be directly removed by a common wet method or a dry adsorption method. COS and CS2Can be converted into H under the action of hydrolysis catalyst2S is convenient for further removal, hydrolysis is a typical double decomposition reaction, the process is independent of electron transfer, normal-temperature hydrolysis is carried out at 30 ~ 100 ℃, medium-temperature hydrolysis is carried out at 200 ~ 250 ℃, and most organic sulfur is converted into H after hydrolysis reaction2S, the reaction formula is as follows: COS + H2O→H2S+CO2；CS2+2H2O→2H2S+CO2(ii) a COS and CS2Or removing by hydrodesulfurization under the action of hydrodesulfurization catalyst at 200 ~ 400 deg.C and 400 deg.C, wherein the hydrogenation reaction is represented by COS + H2→H2S+CO；CS2+4H2→2H2S+CH4。The fine dephosphorization and dearsenification and fine defluorination can adopt corresponding dephosphorization and dearsenification agents and defluorination agents to remove phosphorus, arsenic and fluorine in the gas to be below 0.1 ppm.
The refined purified gas obtained by deep purification can be used for producing various carbon chemical products, such as natural gas, methanol, dimethyl ether, acetic acid, ethylene glycol, and the like.
Example 2:
this embodiment provides a device for purifying yellow phosphorus tail gas.
As shown in fig. 2, the apparatus comprises a washing tower, a pressurizing device, a desulfurizing tower, a fixed bed and an adsorption component which are connected in sequence, wherein the washing tower is provided with a yellow phosphorus tail gas inlet; the fixed bed is filled with a dephosphorizing adsorbent, a steam regeneration system for regenerating the dephosphorizing adsorbent is arranged in the fixed bed, and a steam inlet and a steam outlet which are communicated with the steam regeneration system are arranged on the fixed bed; the adsorption component comprises a temperature swing adsorption bed and a pressure swing adsorption tower set, a primary purified gas outlet is arranged on the temperature swing adsorption bed, the pressure swing adsorption tower set comprises two stages of pressure swing adsorption towers which are connected in series, the primary purified gas outlet is connected with the pressure swing adsorption tower positioned at the first stage, and a fine purified gas outlet is arranged on the pressure swing adsorption tower positioned at the last stage.
The present embodiment will use 20000Nm3The yellow phosphorus tail gas is pressurized to 40kPa by a yellow phosphorus tail gas fan, and then is sent to the working procedures of wet desulphurization, fixed bed dephosphorization elementary substance and temperature swing adsorption to obtain primary purified gas, specifically referring to the step (1) ~ (5) in the example 1, the primary purified gas is pressurized to 2.0MPa and then is sent to the working procedures of two-stage pressure swing adsorption, and the CO in the purified gas is removed by a first-stage pressure swing adsorption tower2And then the CO is purified by fine desulfurization and sent to a second-stage pressure swing adsorption tower, the concentration of the CO can reach more than 98 percent, and the phosphorus, the sulfur, the arsenic and the fluorine are removed to be less than 0.1 ppm. The CO can be used for producing various carbon chemical products, such as natural gas, methanol, dimethyl ether, acetic acid, ethylene glycol and the like.
The above is only the preferred embodiment of the present invention, not to the limitation of the present invention in any form, all the technical matters of the present invention all fall into the protection scope of the present invention to any simple modification and equivalent change of the above embodiments.
Claims (6)
1. The utility model provides a purify device of yellow phosphorus tail gas which characterized in that: the device comprises a washing tower, a desulfurizing tower, a fixed bed and an adsorption component which are sequentially connected, wherein a yellow phosphorus tail gas inlet is formed in the washing tower, a dephosphorizing adsorbent is filled in the fixed bed, the adsorption component comprises a temperature swing adsorption bed, and a primary purified gas outlet is formed in the temperature swing adsorption bed.
2. The apparatus for purifying yellow phosphorus tail gas as claimed in claim 1, wherein: still including the smart desulfurizing tower, smart desulfurization dearsenification tower and the smart defluorinating tower that connect gradually, the smart desulfurizing tower of just purifying gas exit linkage, establish smart purified gas export on the smart defluorinating tower.
3. The apparatus for purifying yellow phosphorus tail gas as claimed in claim 1, wherein: the adsorption component further comprises a pressure swing adsorption tower set, the pressure swing adsorption tower set is composed of two stages of pressure swing adsorption towers which are connected in series, the primary purified gas outlet is connected with the pressure swing adsorption tower positioned at the first stage, and the fine purified gas outlet is arranged on the pressure swing adsorption tower positioned at the last stage.
4. The apparatus for purifying yellow phosphorus tail gas as claimed in claim 1, wherein: a steam regeneration system for regenerating the dephosphorizing adsorbent is arranged in the fixed bed, and a steam inlet and a steam outlet which are communicated with the steam regeneration system are arranged on the fixed bed.
5. The apparatus for purifying yellow phosphorus tail gas as claimed in claim 1, wherein: the number of the temperature swing adsorption beds is at least 5, and each temperature swing adsorption bed is filled with at least two adsorbents.
6. The apparatus for purifying yellow phosphorus tail gas as claimed in claim 1, wherein: and a supercharging device is arranged between the washing tower and the desulfurizing tower.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114191929A (en) * | 2021-12-24 | 2022-03-18 | 常州化工设计院有限公司 | Chemical tail gas treatment process |
| CN114588734A (en) * | 2022-01-28 | 2022-06-07 | 杨光华 | Method for purifying yellow phosphorus tail gas of electric furnace |
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2019
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114191929A (en) * | 2021-12-24 | 2022-03-18 | 常州化工设计院有限公司 | Chemical tail gas treatment process |
| CN114191929B (en) * | 2021-12-24 | 2022-12-06 | 常州化工设计院有限公司 | Chemical tail gas treatment process |
| CN114588734A (en) * | 2022-01-28 | 2022-06-07 | 杨光华 | Method for purifying yellow phosphorus tail gas of electric furnace |
| CN114588734B (en) * | 2022-01-28 | 2023-09-29 | 杨光华 | Method for purifying yellow phosphorus tail gas of electric furnace |
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