CN109173669B - Method for purifying yellow phosphorus tail gas - Google Patents

Method for purifying yellow phosphorus tail gas Download PDF

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CN109173669B
CN109173669B CN201811184445.4A CN201811184445A CN109173669B CN 109173669 B CN109173669 B CN 109173669B CN 201811184445 A CN201811184445 A CN 201811184445A CN 109173669 B CN109173669 B CN 109173669B
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phosphorus
tail gas
sludge
emulsion
yellow phosphorus
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CN109173669A (en
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贾丽娟
李紫珍
宁平
刘天成
王访
高冀芸
刘晨辉
夏福婷
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Yunnan Minzu University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • B01D53/52—Hydrogen sulfide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77—Liquid phase processes
    • B01D53/79—Injecting reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B01D2257/408—Cyanides, e.g. hydrogen cyanide (HCH)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/55—Compounds of silicon, phosphorus, germanium or arsenic
    • B01D2257/553—Compounds comprising hydrogen, e.g. silanes

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Gas Separation By Absorption (AREA)
  • Industrial Gases (AREA)
  • Treating Waste Gases (AREA)

Abstract

The invention provides a method for purifying yellow phosphorus tail gas, belonging to the technical field of waste gas treatment, and the method comprises the steps of mixing phosphorus sludge with water to obtain phosphorus sludge emulsion; and introducing oxygen and the yellow phosphorus tail gas to be treated into the sludge phosphorus emulsion in sequence to carry out oxidation reaction. The invention uses the ozone generated by the phosphorus sludge and oxygen in the liquid phase as the oxidant to cooperate with the Fe contained in the phosphorus sludge emulsion3+Catalytic oxidation of H2S is oxidized and converted into sulfate radical ion, PH3Conversion to PO4 3‑Conversion of HCN to N2And CO2. The operation method is simple; use of waste phosphorus sludge as H in yellow phosphorus tail gas2S、PH3And HCN absorbent, is economical and environment-friendly; the generated reaction product sulfur simple substance, sulfate and phosphate thereof can be recovered, no secondary pollution is caused, and the purification efficiency of the yellow phosphorus tail gas is high. Invention pair H2S and PH3The removal efficiency reaches more than 95 percent, and the purification efficiency of HCN can reach more than 90 percent.

Description

Method for purifying yellow phosphorus tail gas
Technical Field
The invention relates to the technical field of waste gas treatment, in particular to a method for purifying yellow phosphorus tail gas.
Background
The phosphorus chemical industry is an important industry in provinces such as cloud, nobility, Sichuan and Hubei, and Yunnan accounts for more than 50% of yellow phosphorus output in China. The production process of yellow phosphorus is accompanied by a large amount of complex componentsThe generation of toxic and harmful gases is about 2500-3000 Nm per 1t of yellow phosphorus produced3The tail gas of (1) contains 400-1000 mg/Nm of HCN3，PH3750～1200mg/Nm3，H2S 800～8000mg/Nm3And the yellow phosphorus tail gas has complex components and properties, is difficult to purify and recover, is discharged in a combustion mode, not only causes waste of sulfur and carbon resources in the gas, but also seriously pollutes the atmospheric environment. Analysis shows that the resource utilization of the yellow phosphorus tail gas is a fundamental way for enhancing the competitiveness of the yellow phosphorus industry and thoroughly getting rid of the high-pollution and high-energy-consumption cap.
At present, the methods for treating yellow phosphorus tail gas at home and abroad are many and can be divided into an absorption method, a temperature and pressure swing adsorption method and a catalytic oxidation method. Wherein, the temperature and pressure swing adsorption method develops a series of high-selectivity catalysts, and the regeneration is simple; all stages of reactions are mutually linked, so that the heat energy utilization is better; the purified gas not only meets the requirement of oxo synthesis, but also removes toxic gas HCN. However, the technical cost is high, the operation is complicated, and the problem of catalyst life needs to be considered.
Disclosure of Invention
In view of this, the present invention aims to provide a method for purifying yellow phosphorus tail gas, which is simple in operation, low in cost and high in removal efficiency.
The invention provides a method for purifying yellow phosphorus tail gas, which comprises the following steps:
mixing phosphorus sludge with water to obtain phosphorus sludge emulsion;
introducing oxygen and yellow phosphorus tail gas to be treated into the sludge phosphorus emulsion in sequence to carry out oxidation reaction;
the phosphorus sludge is generated in the yellow phosphorus production process; the phosphorus content of the phosphorus sludge is 4-40%, and the phosphorus sludge contains Fe3+The mass content of (A) is 0.83%;
the yellow phosphorus tail gas is the tail gas generated in the yellow phosphorus production process.
Preferably, the solid content of the mud phosphorus emulsion is 5-50 wt%.
Preferably, the amount of the introduced oxygen is such that the oxygen content in the sludge phosphorus emulsion is 5-30%.
Preferably, the content of hydrogen sulfide in the yellow phosphorus tail gas to be treated is 2000-6000 mg/m3The content of hydrogen cyanide is 300-800 mg/m3The content of phosphine is 700-1000 mg/m3。
Preferably, the introduction rate of the yellow phosphorus tail gas to be treated is 0.2-1.0L/min.
Preferably, the volume ratio of the sludge phosphorus emulsion to the yellow phosphorus tail gas to be treated is 2: 5.
Preferably, the temperature of the oxidation reaction is 25-70 ℃, and the pH value of the oxidation reaction is 3.5-7.
Preferably, the device for purifying the yellow phosphorus tail gas comprises a cooler, a dust remover, an absorption reactor and a tail gas alkali washing device which are sequentially connected, wherein an air inlet at the lower end of the absorption reactor is connected with an air pump, and a feed inlet at the upper end of the absorption reactor is sequentially connected with a head tank and a high-pressure pump.
The beneficial technical effects are as follows: the invention provides a method for purifying yellow phosphorus tail gas, which comprises the following steps: mixing phosphorus sludge with water to obtain phosphorus sludge emulsion; introducing oxygen and yellow phosphorus tail gas to be treated into the sludge phosphorus emulsion in sequence to carry out oxidation reaction; the phosphorus sludge is generated in the yellow phosphorus production process; the phosphorus content of the phosphorus sludge is 4-40%, and the phosphorus sludge contains Fe3+The mass content of (A) is 0.83%; the yellow phosphorus tail gas is the tail gas generated in the yellow phosphorus production process. The invention uses the ozone generated by the phosphorus sludge and oxygen in the liquid phase as the oxidant to cooperate with the Fe contained in the phosphorus sludge emulsion3+Catalytic oxidation of H2S is oxidized and converted into sulfate radical ion, PH3Conversion to PO4 3-Conversion of HCN to N2And CO2. The operation method is simple; use of waste phosphorus sludge as H in yellow phosphorus tail gas2S、PH3And HCN absorbent, is economical and environment-friendly; the generated reaction product sulfur simple substance, sulfate and phosphate thereof can be recovered, no secondary pollution is caused, and the purification efficiency of the yellow phosphorus tail gas is high. Experimental data show that the invention is suitable for H2S and PH3The removal efficiency reaches more than 95 percentThe purification efficiency of HCN can reach more than 90 percent.
Drawings
FIG. 1 is a diagram of an apparatus for purifying a yellow phosphorus tail gas according to the present invention;
1-a cooler, 2-a dust remover, 3-an air pump, 4-an absorption reactor, 5-a tail gas alkali cleaner, 6-a high-pressure pump and 7-a high-level tank.
Detailed Description
The invention provides a method for purifying yellow phosphorus tail gas, which comprises the following steps:
mixing phosphorus sludge with water to obtain phosphorus sludge emulsion;
introducing oxygen and yellow phosphorus tail gas to be treated into the sludge phosphorus emulsion in sequence to carry out oxidation reaction;
the phosphorus sludge is generated in the yellow phosphorus production process; the phosphorus content of the phosphorus sludge is 4-40%, and the phosphorus sludge contains Fe3+The mass content of (A) is 0.83%;
the yellow phosphorus tail gas is the tail gas generated in the yellow phosphorus production process.
The invention mixes phosphorus sludge with water to obtain phosphorus sludge emulsion.
In the invention, the phosphorus content in the phosphorus sludge is preferably 10-40%, and more preferably 20-40%.
In the invention, Fe in the phosphorus sludge3+The content of (b) is preferably 0.5% to 0.9%, more preferably 0.7% to 0.9%.
In the invention, the solid content of the phosphorous slurry emulsion is preferably 5-50 wt%, more preferably 10-40 wt%, and most preferably 20-30 wt%.
After the sludge phosphorus emulsion is obtained, the invention sequentially introduces oxygen and yellow phosphorus tail gas to be treated into the sludge phosphorus emulsion, wherein the yellow phosphorus tail gas to be treated is tail gas generated in the process of producing yellow phosphorus.
In the present invention, the oxygen is preferably introduced in the form of air.
In the invention, the oxygen is introduced in an amount such that the oxygen content in the sludge phosphorus emulsion is preferably 5-30%, more preferably 10-20%, and most preferably 15%. In the invention, the oxygen content in the mud phosphorus emulsion is measured by a flue gas analyzer.
In the invention, the content of hydrogen sulfide in the gas to be treated is preferably 2000-6000 mg/m3More preferably 3000-5000 mg/m3(ii) a The content of hydrogen cyanide is preferably 300-800 mg/m3More preferably 400 to 700mg/m3Most preferably 500 to 600mg/m3(ii) a The content of phosphine is preferably 700-1000 mg/m3More preferably 800 to 900mg/m3Most preferably 850 to 880mg/m3。
In the invention, the introduction rate of the yellow phosphorus tail gas to be treated is preferably 0.2-1.0L/min, and more preferably 0.5-0.8L/min.
In the invention, the volume ratio of the sludge phosphorus emulsion to the yellow phosphorus tail gas to be treated is preferably 2: 5.
The invention uses the ozone induced by phosphorus sludge and oxygen as oxidant to cooperate with Fe contained in the phosphorus sludge emulsion3+Catalytic oxidation of H2S is oxidized and converted into sulfate radical ion, PH3Conversion to PO4 3-Conversion of HCN to N2And CO2。
In the invention, the yellow phosphorus tail gas to be treated preferably comprises cooling and dust removal in sequence before being introduced.
The cooling method of the present invention is not particularly limited, and a cooling method known to those skilled in the art may be used.
The method for removing dust in the present invention is not particularly limited, and a dust removing method known to those skilled in the art may be selected.
In the invention, the temperature of the oxidation reaction is preferably 25-70 ℃, and more preferably 30-50 ℃; the pH value of the oxidation reaction is preferably 3.5-7, and more preferably 5-6.
In the invention, the invalid sludge phosphorus emulsion obtained after the oxidation reaction can be further recycled.
In the invention, the device for purifying the yellow phosphorus tail gas comprises a cooler, a dust remover, an absorption reactor and a tail gas alkali washing device which are sequentially connected, wherein an air inlet at the lower end of the absorption reactor is connected with an air pump, and a feed inlet at the upper end of the absorption reactor is sequentially connected with a head tank and a high-pressure pump. The device for purifying the yellow phosphorus tail gas is specifically shown in figure 1.
In the invention, the specific operation of purifying the yellow phosphorus tail gas is as follows: air is blown into an absorption reactor 4 by an air pump 3 to fully react with elemental phosphorus and oxygen in the sludge phosphorus emulsion to generate ozone, yellow phosphorus tail gas to be treated from an emission source is cooled by a cooler 1 and dedusted by a deduster 2 and then enters the absorption reactor 4 to carry out oxidation reaction, gas after the absorption reaction is dried by a tail gas alkali scrubber 5 and then is exhausted, the sludge phosphorus emulsion is filled in the absorption reactor 4, the invalid emulsion is transferred to the next workshop by a pipeline with a control valve at the bottom to be recycled, the sludge phosphorus emulsion is pumped into an elevated tank 7 by a high-pressure pump 6 and then continuously replenished with fresh slurry to enter the absorption reactor 4, and the cooler 1 can utilize the heat energy thereof in a heat exchange manner to reduce energy waste.
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
The phosphorus content in the phosphorus mud is detected to be 45 percent and Fe by adopting 0.5g of phosphorus mud of a yellow phosphorus factory in Yunnan province3+Preparing 40mL of emulsion with the content of 0.83 percent, placing the emulsion in an absorption reactor, introducing air, introducing the air to ensure that the oxygen content in the phosphorus sludge is 20 percent, and then introducing H2S、PH3And HCN (H in mock gas)2The concentration of S gas is 1100mg/m3、PH3The gas concentration is 800mg/m3The concentration of HCN gas is 600mg/m3) The airflow rate is 0.3L/min, the reaction time is 350min, the temperature of the absorption reactor is controlled at 40 ℃, and the experimental result is H2S removal rate of 98% and PH3The removal rate of 87 percent and the removal rate of 83 percent of HCN can last for 270 min.
Example 2
The phosphorus content in the phosphorus mud is detected to be 45 percent and Fe by adopting 0.7g of phosphorus mud of a yellow phosphorus factory in Yunnan province3+The content of the phosphorus mud is 0.83 percentMaking into 40mL emulsion, placing in an absorption reactor, introducing air, introducing oxygen to make the oxygen content in the phosphorus sludge be 20%, and introducing H2S、PH3And HCN (H in mock gas)2The concentration of S gas is 1100mg/m3、PH3The gas concentration is 800mg/m3The concentration of HCN gas is 600mg/m3) The airflow rate is 0.3L/min, the reaction time is 350min, the temperature of the absorption reactor is controlled at 60 ℃, and the experimental result is H2S removal rate of 99% and PH3The time for removing 96 percent of HCN and 93 percent of HCN can last for 300 min.
Example 3
The phosphorus content in the phosphorus mud is detected to be 45 percent and Fe by adopting 0.5g of phosphorus mud of a yellow phosphorus factory in Yunnan province3+The content is 0.83 percent, the phosphorus sludge is prepared into 40mL of emulsion, the emulsion is placed in an absorption reactor, air is introduced, the mass content of oxygen in the phosphorus sludge is 15 percent after the air is introduced, and then H is introduced2S、PH3And HCN (H in mock gas)2The concentration of S gas is 1100mg/m3、PH3The gas concentration is 800mg/m3The concentration of HCN gas is 600mg/m3) The airflow rate is 0.7L/min, the reaction time is 350min, the temperature of the absorption reactor is controlled at 70 ℃, and the experimental result is H2S removal rate of 94% and PH3The removal rate of 83 percent and the removal rate of HCN of 79 percent can last for 250 min.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (8)

1. A method for purifying yellow phosphorus tail gas comprises the following steps:
mixing phosphorus sludge with water to obtain phosphorus sludge emulsion;
introducing oxygen and yellow phosphorus tail gas to be treated into the sludge phosphorus emulsion in sequence to carry out oxidation reaction; the pH value of the oxidation reaction is 3.5-7;
the sludge phosphorus is rawSludge phosphorus generated in the process of producing yellow phosphorus; the phosphorus content in the phosphorus sludge is 4-40%, and the phosphorus sludge contains Fe3+The mass content of (A) is 0.83%;
the yellow phosphorus tail gas is the tail gas generated in the yellow phosphorus production process.
2. A method according to claim 1, wherein the sludge phosphorus emulsion has a solids content of 5 to 50 wt.%.
3. The method as claimed in claim 1, wherein the oxygen is introduced in an amount such that the content of oxygen in the slurry phosphorus emulsion is 5-30%.
4. The method according to claim 1, wherein the content of hydrogen sulfide in the yellow phosphorus tail gas to be treated is 2000-6000 mg/m3The content of hydrogen cyanide is 300-800 mg/m3The content of phosphine is 700-1000 mg/m3。
5. The method as claimed in claim 1, wherein the introduction rate of the yellow phosphorus tail gas to be treated is 0.2-1.0L/min.
6. The method according to claim 1, 4 or 5, wherein the volume ratio of the sludge phosphorus emulsion to the yellow phosphorus tail gas to be treated is 2: 5.
7. The method of claim 1, wherein the temperature of the oxidation reaction is between 25 ℃ and 70 ℃.
8. The method according to claim 1, wherein the device for purifying the yellow phosphorus tail gas comprises a cooler, a dust remover, an absorption reactor and a tail gas alkali scrubber which are sequentially connected, wherein an air inlet at the lower end of the absorption reactor is connected with an air pump, and an upper end feed inlet of the absorption reactor is sequentially connected with a head tank and a high-pressure pump.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110102180A (en) * 2019-06-21 2019-08-09 云南民族大学 A kind of method of mud Emulphors turbid liquid phase catalytic oxidation simultaneous SO_2 and NO removal
CN110304608B (en) * 2019-07-02 2023-04-07 昆明理工大学 Method for preparing ozone and by-product phosphoric acid by liquid-phase oxidation of phosphorus sludge
CN111992028A (en) * 2020-08-19 2020-11-27 昆明理工大学 Additive for enhancing hydrogen sulfide removal of yellow phosphorus slurry and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101024140A (en) * 2007-01-15 2007-08-29 左建国 Method for purifying phosphor tail-gas
CN104307365A (en) * 2014-10-17 2015-01-28 陕西华陆化工环保有限公司 Cleaning method of hydrogen sulfide gas
CN108568202A (en) * 2017-03-09 2018-09-25 云南民族大学 A kind of method of mud phosphorus removing nitrogen oxides

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101024140A (en) * 2007-01-15 2007-08-29 左建国 Method for purifying phosphor tail-gas
CN104307365A (en) * 2014-10-17 2015-01-28 陕西华陆化工环保有限公司 Cleaning method of hydrogen sulfide gas
CN108568202A (en) * 2017-03-09 2018-09-25 云南民族大学 A kind of method of mud phosphorus removing nitrogen oxides

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