CN113578004A - SO in activated coke desorption gasxCollecting device and collecting method - Google Patents

SO in activated coke desorption gasxCollecting device and collecting method Download PDF

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Publication number
CN113578004A
CN113578004A CN202110861505.7A CN202110861505A CN113578004A CN 113578004 A CN113578004 A CN 113578004A CN 202110861505 A CN202110861505 A CN 202110861505A CN 113578004 A CN113578004 A CN 113578004A
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China
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washing bottle
gas washing
gas
sulfuric acid
acid mist
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CN202110861505.7A
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Inventor
熊劲
邵雁
向浩
刘子豪
姜明明
刘颖
史记熙
雷配双
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China City Environment Protection Engineering Ltd
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China City Environment Protection Engineering Ltd
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Priority to CN202110861505.7A priority Critical patent/CN113578004A/en
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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
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • B01D53/50—Sulfur oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2205—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with filters
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/10—Oxidants
    • B01D2251/106—Peroxides
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • G01N2001/2217—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption using a liquid

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
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  • Molecular Biology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention provides SO in active coke desorption gasxThe collection system of (1) comprises a first gas washing bottle, a second gas washing bottle and a filtering piece for intercepting sulfuric acid mist, wherein an outlet of an active coke analysis device is communicated with an inlet of the filtering piece after sequentially passing through the first gas washing bottle and the second gas washing bottle, the active coke analysis device is communicated with the first gas washing bottle, the first gas washing bottle and the second gas washing bottle, and the second gas washing bottle is communicated with the filtering piece through an anti-corrosion pipeline component. The invention also provides SO in the active coke desorption gasxThe collection method of (1). The quartz sintering filter ball is additionally arranged at the outlet of the second gas washing bottle to trap escaping sulfuric acid mist, and the quartz sintering filter ball is adoptedThe technology can completely capture SO in the analytic gasxAnd the accuracy of the desulfurization value test is improved. The connecting pipeline and the joint are made of corrosion-resistant PTFE/PFA materials, SO that SO is eliminated3Losses in the piping.

Description

SO in activated coke desorption gasxCollecting device and collecting method
Technical Field
The invention relates to the field of flue gas sampling, in particular to activated coke desorption gas SOxThe collecting device and the collecting method.
Background
The desulfurization and denitrification technology of the active coke utilizes the adsorption and catalysis functions of the active coke to integrally remove SO in the flue gas2、NOxAnd mercury, dioxin and other multiple pollutants. The active coke desulfurization and denitrification technology is clean, efficient, low in energy consumption and capable of recycling by-products, and is a flue gas purification technology with great development potential. The core material of the technology is porous active coke made of coal as a raw material, and in the desulfurization and denitrification process, the active coke is aligned to SO through internal micropores in an adsorption tower2Performing physical adsorption and chemical adsorption, and catalyzing NO by surface active groupxAnd NH3SCR reaction to generate N2. After the adsorption is saturated, the active coke enters a regeneration tower, the adsorbate is removed at a high temperature of about 400 ℃, the adsorption capacity of the active coke is recovered, and the active coke enters the adsorption tower again for next adsorption.
The national standard "desulfurization and denitrification coal granular activated carbon test method part 4 desulfurization value" (GB/T30202.4-2013) specifies a test method of the desulfurization value of activated coke. And adsorbing the mixed gas of sulfur dioxide, water vapor, oxygen and nitrogen by the pretreated sample under a certain condition, introducing nitrogen for analysis after the sulfur dioxide is adsorbed in a saturated manner, and calculating the desulfurization value of the active coke according to the analyzed amount of the sulfur dioxide. Wherein the SO in the desorption gas2The collection mode of the device is that two 3L absorption bottles are connected in series and filled with 2L hydrogen peroxide solution with the mass fraction of 3% for absorption. During the actual process of active coke desorption, white mist is generated in the absorption bottle, and part of the white mist escapes from the outlet of the second absorption bottle. White mist is SO3The submicron acid mist generated by the combination of the gas and the water vapor in the absorption bottle is not easy to settle and diffuse, so that the submicron acid mist is difficult to be absorbed by the absorption liquid and finally partially escapes. Illustrating that the active coke decomposition gas not only contains SO2Also contains a certain amount of SO3The existing absorption mode can not completely collect SO3And the rubber connecting pipe in the collecting device consumes part of SO3Ultimately resulting in lower test results for desulfurization values.
Therefore, it is necessary to design a new active coke decomposition gas containing SOxTo overcome the above problems.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the activated coke desorption gas for SOxAiming at the problem that the existing active coke desorption gas absorption device can not completely collect SO3And the problem that the desulfurization value test value is low due to the fact that the connecting pipeline is not corrosion-resistant, and the SO is completely collected by using the corrosion-resistant pipeline and adding a quartz sintering filter at the tail part of the gas washing bottlexThe accuracy of desulfurization value test is improved, and at least partial problems in the prior art are solved.
The invention is realized by the following steps:
the invention provides SO in active coke desorption gasxThe collection device comprises a first gas washing bottle, a second gas washing bottle and a filtering piece for intercepting sulfuric acid mist, wherein an outlet of the active coke analysis device is communicated with an inlet of the filtering piece after sequentially passing through the first gas washing bottle and the second gas washing bottle.
Preferably, the active coke analysis device is communicated with the first gas washing bottle, the first gas washing bottle is communicated with the second gas washing bottle, and the second gas washing bottle is communicated with the filtering element through an anti-corrosion pipeline assembly.
Preferably, the anti-corrosion pipeline assembly comprises an anti-corrosion pipeline, and two ends of the pipeline are respectively communicated with an anti-corrosion clamping sleeve head.
Preferably, the pipeline is a PTFE pipe or a PFA pipe.
Preferably, the clamping sleeve joint is a PTFE clamping sleeve joint or a PFA clamping sleeve joint.
Preferably, the tube is a stretchable helical tube.
Preferably, the filter element is a quartz sintered filter ball.
Preferably, the direction from the inlet of the quartz sintered filter ball to the outlet of the quartz sintered filter ball is the same as the direction in which the sulfuric acid mist flows into the quartz sintered filter ball.
The invention also provides SO in the active coke desorption gasxThe collection method comprises the following steps: the desorption gas from the active coke desorption device sequentially passes through a first gas washing bottle, a second gas washing bottle and a quartz sintering filter ball, and SO is2A part of SO absorbed in the first gas washing bottle and a part of SO not absorbed by the first gas washing bottle2Is completely absorbed after entering a second gas washing bottle, and absorbed SO2Generating stable sulfate ions under the oxidation action of hydrogen peroxide; SO (SO)3The sulfuric acid mist and the water vapor are combined in the first gas washing bottle to form submicron-grade sulfuric acid mist, one part of the sulfuric acid mist is absorbed in the first gas washing bottle, one part of the sulfuric acid mist enters the second gas washing bottle along with the air flow to be absorbed, the sulfuric acid mist which is not absorbed by the second gas washing bottle continues to enter the quartz sintering filter ball along with the air flow, and the whole sulfuric acid mist is intercepted in a sintering filter element of the quartz sintering filter ball; after the collection is finished, besides collecting hydrogen peroxide absorption liquid in the first gas washing bottle and the second gas washing bottle, deionized water is needed to be used for cleaning the quartz sintered filter ball, all the ferrule joints and the inner wall of the pipeline, and cleaning liquid is collected, wherein the total amount of sulfate radicals in the absorption liquid and the cleaning liquid is SO in the analysis gasxTotal amount of the components.
The invention has the following beneficial effects:
the existing active coke desorption gas absorption device only considers the SO2The absorption is carried out by adopting two gas washing bottles which are connected in series and are filled with hydrogen peroxide solution, and the desorption device is used for dischargingThe port is connected with the inlet of the gas washing bottle and the two gas washing bottles by silica gel hoses. The actual analysis gas simultaneously contains SO with strong corrosiveness3Two problems result, one is SO3Reacts with the silicone tube to cause the silicone tube to age and even damage, and simultaneously consumes part of SO3(ii) a Second is SO3Reacts with water vapor in the gas washing bottle to generate submicron-grade sulfuric acid mist which is not easy to settle and diffuse, so that the submicron-grade sulfuric acid mist is difficult to be absorbed by absorption liquid and partially escapes. The net result is a lower desulfurization value for the test. Aiming at the problems, the invention has two improvements, one is that the connecting pipeline and the joint are all made of corrosion-resistant PTFE/PFA materials, SO that SO is eliminated3Losses in the piping; and secondly, a quartz sintering filter ball is added at the outlet of the second gas washing bottle to capture escaping sulfuric acid mist. The technique can completely capture SO in the analytic gasxAnd the accuracy of the desulfurization value test is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 shows SO in the gas from active coke decomposition according to an embodiment of the present inventionxSchematic view of the collecting device.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, an embodiment of the present invention provides a method for resolving SO in gas by using activated cokexIs collected and putThe device comprises a first gas washing bottle 4, a second gas washing bottle 5 and a filtering piece for intercepting sulfuric acid mist, wherein the first gas washing bottle 4 and the second gas washing bottle 5 are both filled with a gas for absorbing SO2The filtering piece is a quartz sintering filtering ball 3, and the outlet of the active coke analysis device is communicated with the inlet of the filtering piece after sequentially passing through the first gas washing bottle 4 and the second gas washing bottle 5.
And a quartz sintering filter ball 3 is added at the outlet of the second gas washing bottle 5 to capture the escaped sulfuric acid mist. The technique can completely capture SO in the analytic gasxAnd the accuracy of the desulfurization value test is improved.
The active coke analysis device is communicated with the first gas washing bottle 4, the first gas washing bottle 4 is communicated with the second gas washing bottle 5, and the second gas washing bottle 5 is communicated with the filtering piece through an anti-corrosion pipeline assembly. The anti-corrosion pipeline assembly comprises an anti-corrosion pipeline 2, and two ends of the pipeline 2 are respectively communicated with an anti-corrosion clamping sleeve head 1. The pipeline 2 is a PTFE pipe or a PFA pipe. The clamping sleeve head 1 is a PTFE (polytetrafluoroethylene) sleeve joint or a PFA (Polytetrafluoroethylene) sleeve joint. The connecting pipeline and the joint are made of corrosion-resistant PTFE/PFA materials, SO that SO is eliminated3Losses in the piping. The tube 2 is a stretchable helical tube.
The direction from the inlet of the quartz sintering filter ball 3 to the outlet of the quartz sintering filter ball 3 is the same as the direction of the sulfuric acid mist flowing into the quartz sintering filter ball 3.
The embodiment of the invention also provides SO in the activated coke desorption gasxThe collection method comprises the following steps: the desorption gas from the active coke desorption device sequentially passes through a first gas washing bottle 4, a second gas washing bottle 5 and a quartz sintering filter ball 3, SO2A part of the SO absorbed in the first scrubbing cylinder 4 and a part of the SO not absorbed in the first scrubbing cylinder 42Is completely absorbed after entering the second gas washing bottle 5, and absorbed SO2Generating stable sulfate ions under the oxidation action of hydrogen peroxide; SO (SO)3The sulfuric acid mist in submicron order is formed by combining with the water vapor in the first gas washing bottle 4, one part of the sulfuric acid mist is absorbed in the first gas washing bottle 4, one part of the sulfuric acid mist enters the second gas washing bottle 5 along with the air flow to be absorbed, and the sulfuric acid mist which is not absorbed by the second gas washing bottle 5 is absorbed sequentiallyThe sulfuric acid mist enters the quartz sintering filter ball 3 along with the air flow, and the sulfuric acid mist is all intercepted in a sintering filter core of the quartz sintering filter ball 3; after the collection is finished, besides collecting hydrogen peroxide absorption liquid in the first gas washing bottle 4 and the second gas washing bottle 5, deionized water is needed to be used for cleaning the quartz sintered filter ball, all the ferrule joints 1 and the inner wall of the pipeline 2, and cleaning liquid is collected, wherein the total amount of sulfate radicals in the absorption liquid and the cleaning liquid is SO in the analysis gasxTotal amount of the components.
The device consists of a first gas washing bottle 4, a second gas washing bottle 5 and a quartz sintering filter ball 3. The clamp sleeve joint 1 and the pipeline 2 which are made of PTFE/PFA materials are connected between the outlet of the analysis device and the inlet of the first gas washing bottle 4, between the outlet of the first gas washing bottle 4 and the inlet of the second gas washing bottle 5 and between the outlet of the second gas washing bottle 5 and the inlet of the quartz sintering filter ball 3, and preferably, the pipeline 2 is made into a spiral pipe style which can be stretched. The gas washing bottle is filled with hydrogen peroxide solution 6 for absorbing SO2. The filter element specification of the quartz sintered filter ball 3 is above G3, which is used for completely collecting escaped sulfuric acid mist, and preferably, the quartz sintered filter ball 3 is vertically arranged.
The desorption gas from the desorption device passes through a first gas washing bottle 4, a second gas washing bottle 5 and a quartz sintering filter ball 3. SO (SO)2Is mainly absorbed in the first scrubbing cylinder 4, and a small part of the SO not absorbed by the first scrubbing cylinder 42Is completely absorbed after entering the second gas washing bottle 5, and absorbed SO2Stable sulfate ions are generated under the oxidation action of hydrogen peroxide. SO (SO)3The sulfuric acid mist of submicron order is formed by combining with water vapor in the first gas washing bottle 4, a small part of the sulfuric acid mist is absorbed in the first gas washing bottle 4, most of the sulfuric acid mist enters the second gas washing bottle 5 along with the air flow, the small part of the sulfuric acid mist is absorbed at the place, most of the sulfuric acid mist continues to enter the quartz sintering filter ball 3 along with the air flow, and all the sulfuric acid mist is intercepted in a sintering filter core of the quartz sintering filter ball 3. After the collection is finished, besides collecting the absorption liquid in the first gas washing bottle 4 and the second gas washing bottle 5, the quartz sintered filter ball, all the ferrule joints 1 and the inner wall of the pipeline 2 need to be cleaned by deionized water, and the cleaning liquid is collected, wherein the total amount of sulfate radicals in the absorption liquid and the cleaning liquid is SO in the analysis gasxTotal amount of the components.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (9)

1. SO in activated coke desorption gasxThe collection system, its characterized in that: including first gas washing bottle, second gas washing bottle and one hold back the filter piece of sulfuric acid mist, the export of active burnt analytical equipment loop through behind first gas washing bottle, the second gas washing bottle with the entry intercommunication of filter piece.
2. SO in the active coke analysis gas as defined in claim 1xThe collection system, its characterized in that: the active coke analysis device is communicated with the first gas washing bottle, the first gas washing bottle is communicated with the second gas washing bottle, and the second gas washing bottle is communicated with the filtering piece through an anti-corrosion pipeline assembly.
3. SO in the active coke analysis gas as defined in claim 2xThe collection system, its characterized in that: the anti-corrosion pipeline assembly comprises an anti-corrosion pipeline, and two ends of the pipeline are respectively communicated with an anti-corrosion clamping sleeve head.
4. SO in the active coke analysis gas as defined in claim 3xThe collection system, its characterized in that: the pipeline is a PTFE pipe or a PFA pipe.
5. SO in the active coke analysis gas as defined in claim 3xThe collection system, its characterized in that: the clamping sleeve head is a PTFE (Polytetrafluoroethylene) sleeve joint or a PFA (Polytetrafluoroethylene) sleeve joint.
6. SO in the active coke analysis gas as defined in claim 3xThe collection system, its characterized in that: the tube is a stretchable helical tube.
7. SO in the active coke analysis gas as defined in claim 1xThe collection system, its characterized in that: the filter element is a quartz sintered filter ball.
8. SO in the active coke analysis gas as claimed in claim 7xThe collection system, its characterized in that: the direction from the quartz sintering filter ball inlet to the quartz sintering filter ball outlet is the same as the direction in which the sulfuric acid mist flows into the quartz sintering filter ball.
9. SO in activated coke desorption gasxThe collection method is characterized in that: the desorption gas from the active coke desorption device sequentially passes through a first gas washing bottle, a second gas washing bottle and a quartz sintering filter ball, and SO is2A part of SO absorbed in the first gas washing bottle and a part of SO not absorbed by the first gas washing bottle2Is completely absorbed after entering a second gas washing bottle, and absorbed SO2Generating stable sulfate ions under the oxidation action of hydrogen peroxide; SO (SO)3The sulfuric acid mist and the water vapor are combined in the first gas washing bottle to form submicron-grade sulfuric acid mist, one part of the sulfuric acid mist is absorbed in the first gas washing bottle, one part of the sulfuric acid mist enters the second gas washing bottle along with the air flow to be absorbed, the sulfuric acid mist which is not absorbed by the second gas washing bottle continues to enter the quartz sintering filter ball along with the air flow, and the whole sulfuric acid mist is intercepted in a sintering filter element of the quartz sintering filter ball; after the collection is finished, besides collecting hydrogen peroxide absorption liquid in the first gas washing bottle and the second gas washing bottle, deionized water is needed to be used for cleaning the quartz sintered filter ball, all the ferrule joints and the inner wall of the pipeline, and cleaning liquid is collected, wherein the total amount of sulfate radicals in the absorption liquid and the cleaning liquid is SO in the analysis gasxTotal amount of the components.
CN202110861505.7A 2021-07-29 2021-07-29 SO in activated coke desorption gasxCollecting device and collecting method Pending CN113578004A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114217010A (en) * 2021-11-29 2022-03-22 北京首钢股份有限公司 Analytic system and method for testing analytic effect of activated carbon for desulfurization and denitrification

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114217010A (en) * 2021-11-29 2022-03-22 北京首钢股份有限公司 Analytic system and method for testing analytic effect of activated carbon for desulfurization and denitrification

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