CN110465110A - A kind of gas phase arsenic quantitatively occurs and adsorbent equipment - Google Patents
A kind of gas phase arsenic quantitatively occurs and adsorbent equipment Download PDFInfo
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- CN110465110A CN110465110A CN201910396350.7A CN201910396350A CN110465110A CN 110465110 A CN110465110 A CN 110465110A CN 201910396350 A CN201910396350 A CN 201910396350A CN 110465110 A CN110465110 A CN 110465110A
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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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
- B01D53/04—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 by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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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
- B01D53/14—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 by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
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Abstract
The present invention provides a kind of devices and its application method that gas phase arsenic quantitatively can occurs and adsorbed, and belong to arsenic in coal-fired flue-gas and control correlative technology field.It mainly include gas phase arsenic generating device, adsorbent equipment and device for absorbing tail gas.The carrier gas for flowing through mass flowmenter is preheated by oil bath, it carries gas phase arsenic and reaction gas is mixed to form air-flow containing arsenic, this air-flow containing arsenic passes through adsorbent bed from bottom to top and adsorbent occurs adsorption reaction, unadsorbed gas phase arsenic and carrier gas and is discharged after the washing of tail gas absorption bottle.The present apparatus generates gas phase arsenic by the way of solid sublimation, solves prior art bring vapor or O2It influences；Gas phase arsenic generator uses " W " configuration and is placed in oil bath pan and heats, and realizes the uniform mixing of air-flow, and carried out preferable preheating to inlet air flow；Pass through the summation of arsenic content in sample waste and adsorbent in comparison generating device and absorbing liquid, it is ensured that total arsenic amount balance reduces experimental error.
Description
Technical field
The invention belongs to arsenic in coal-fired flue-gas to control correlative technology field, especially be that by continuing quantitatively for gas phase arsenic
Occur, and guarantees to influence in adsorption process without other factors, gas-tight.
Background technique
Arsenic is the metalloid substance of discharge during coal utilization, and arsenical is carcinogenic harmfulness in current natural environment
One of maximum substance, Long Term Contact can cause cytotoxic and capillary toxicosis, it is also possible to lead to lung cancer, cutaneum carcinoma etc..
With the aggravation of mankind's activity, the discharge amount of arsenic is gradually increased, and has been caused both at home and abroad to the emission control of arsenic in industrial smoke
Extensive concern.Adsorber technologies are current research than wide, efficient flue gas arsenic removing method, the solid in coal fired power plant flue
The addition of adsorbent can condense for gaseous state arsenide and provide surface area, be conducive to the physics and chemisorption of arsenic.It studies more
Absorption arsenic removal the active iron processes of method, aluminum oxide method, active carbon adsorption, load and modified ion-exchange-resin process
Deng.
Currently, being in laboratory stage mostly using the removing research that adsorbent carries out arsenic.For example, document " coal-fired flue-gas
The absorption and control mechanism study of middle arsenic " in using hydride generator generate AsH3(g), then with O2Reaction generates As2O3(g)
Gas, therefore flow through in the air-flow containing arsenic of adsorbent bed and may contain O2, experiment precision is reduced, in addition, this device is not set
Device for absorbing tail gas is set, the gas phase arsenic leaked in experimentation may cause damages to operator and atmosphere；Document
《Experimental and Mechanism Study of Gas-Phase Arsenic Adsorption Over Fe2O3/
γ-Al2O3Sorbent in Oxy-Fuel Combustion Flue Gas " involved in device using heating arsenic standard liquid
The method for generating gas phase arsenic, not can avoid the influence that vapor adsorbs gas phase arsenic in reaction process, meanwhile, using needle injection
The problems such as arsenic standard liquid may cause gas phase arsenic to be unevenly distributed in furnace；Document " in coal-fired flue-gas the existence form of arsenic and its
Adsorption law research in molecular sieve " it is middle using arsenic acid (H3AsO4) arsenic source is used as to carry out decomposition vaporization, it is converted into thermally labile
The As of property2O5, and then oxygen loss generates As4O6, the method can not avoid O2Influence to adsorption process.
Summary of the invention
For the disadvantages described above and Improvement requirement of the prior art, the present invention provides a kind of gas phase arsenic quantitatively to occur and adsorb
Device, this method quantitatively generate gas phase arsenic by heating sublimation arsenic trioxide powder, mixed with reaction gas under carrier gas carrying
It closes into adsorbent equipment, unadsorbed gas phase arsenic and carrier gas and is discharged after the washing of tail gas absorption bottle.This method not only solves
Vapor, O in adsorption process2Etc. factors influence, while also avoiding arsenic leakage, the condensation problem in pipeline.
In order to achieve the above object, the present invention provides following technical schemes, it is characterised in that:
The experimental provision consists of three parts, gas phase arsenic generating device, adsorbent equipment and device for absorbing tail gas.Gas phase arsenic
Generating device includes oil bath pan and gas phase arsenic generator, is adjusted by the coupling of carrier gas flux and oil temperature and realizes quantifying for gas phase arsenic
Occur；Adsorbent equipment mainly includes crystal reaction tube, the adsorbent bed in crystal reaction tube and electric furnace, temperature controller,
Adsorbent bed is located at the middle position of electric furnace, and temperature controller adjusts adsorption temp by control electric furnace temperature to meet reality
Test requirement；Air-flow containing arsenic flows through adsorbent bed from bottom to top and is adsorbed by adsorbent, and unadsorbed gas phase arsenic and carrier gas are inhaled through tail gas
It is discharged after receiving apparatus washing.
In general, technical solution proposed by the present invention compared with prior art, has the advantage that
1. passing through heating As2O3Powder generates gas phase arsenic, and is carried along into adsorbent equipment by carrier gas, solves and utilizes arsenic mark
Liquid influences as occurring source bring vapor and heats arsenic acid (H3AsO4) caused by O2It influences；Pass through oil temperature and carrier gas flux
Coupling adjust and realize the quantitative generation of gas phase arsenic.
2. gas phase arsenic generator uses " W " configuration and is placed in oil bath pan and heats, the uniform mixing of air-flow is realized, and right
Inlet air flow has carried out preferable preheating；Gas phase arsenic generator and crystal reaction tube coupling part are heated using heat tracing pipe, are avoided
Condensation of the gas phase arsenic in tube wall.
3. adjusting absorption bed temperature by control electric furnace temperature, the adsorption reaction under different temperatures is realized；Absorption
Bed can be removed before and after experiment, convenient for the pick-and-place and weighing of adsorbent, strengthen the essence to arsenic content in adsorbent
Degree.
4. the addition of absorbing liquid had both avoided the harm for not absorbing gas to human health, while can also be inhaled by measurement
Arsenic content in liquid is received, is compared in conjunction with adsorbent institute arsenic-adsorbing amount with sample losing quantity, it is ensured that total arsenic amount balance reduces experiment
Error.
A kind of gas phase arsenic occurs and the application method of adsorbent equipment, includes the following steps:
Step 1: crystal reaction tube (17), gas phase arsenic generator (10) are connected and cover upper heat tracing pipe in designated position
(13), it is respectively placed in electric furnace (14) furnace chamber, oil bath pan (11), according to setting electric furnace (14), oil bath needed for experiment
Pot (11) and heat tracing pipe (13) temperature, is denoted as t respectively1、t2、t3, unit is DEG C；
Step 2: selection experiment is sorbent used, weighs its quality and is denoted as m1, adsorbent is evenly laid out in adsorbent bed
(16) on；
Step 3: it weighs crucible (8) quality and is denoted as m2, a certain amount of arsenic trioxide powder is added thereto, weighs sample
Product and crucible (8) gross mass are denoted as m3, then added sample quality is m3-m2, unit g；
Step 4: 5%HNO is prepared3/ 10%H2O2Solution measures the 100mL solution respectively and pours into two absorption bottles, adopts
Two absorption bottles are connected with hose；
Step 5: after electric furnace (14), oil bath pan (11) and heat tracing pipe (13) temperature are stablized, the earthenware of sample will be housed
Crucible (8) is placed in gas phase arsenic generator (10), and adsorbent bed (16) is placed in fixed position inside crystal reaction tube (17)；
Step 6: connection carrier gas is opened mass flowmenter (5,6), flow is denoted as F respectively1、F2, unit mL/min；
Step 7: being first shut off oil bath pan (11) after the reaction time needed for reaching, then successively close heat tracing pipe (13),
Electric furnace (14) after keeping carrier gas high-temperature blowing 15min, closes air valve and mass flowmenter (5,6).
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention.
1,2. carrier gas gas cylinder in figure, 3,4. manually-operated gates, 5,6. mass flowmenters, 7. crossover subs, 8. crucibles, 9. quartz
Sieve plate, 10. gas phase arsenic generators, 11. oil bath pans, 12. frosted interfaces, 13. heat tracing pipes, 14. electric furnaces, 15. temperature controllers,
16. adsorbent bed, 17. crystal reaction tubes, 18. crossover subs, 19. tail gas absorption bottles
Specific embodiment
To be more clear advantages of the present invention and technical solution, with reference to the accompanying drawing and specific embodiment is to the present invention
Technical solution be further described.
In Fig. 1, sample powder is located in crucible (8), and quartzy sieve plate (9) had not only played the role of support crucible (9), but also
It ensure that the sample for flowing through adsorbent equipment is gas phase；Gas phase arsenic generator (10) is located in oil bath pan (11), by oil bath plus
Heat realizes the distillation of arsenic trioxide, to generate stable air-flow containing arsenic；Small-sized electrical heating furnace (14) is placed vertically, adsorbent bed
(16) it is located in crystal reaction tube (17) and is located at furnace body middle position, adjusts suction by controlling electric furnace (14) temperature
Attached bed (16) temperature, realizes the adsorption reaction under different temperatures；Crystal reaction tube (17) and gas phase arsenic generator (10) use frosted
Interface (12) is connected and is heated by heat tracing pipe (13), avoids condensation of the gas phase arsenic in pipeline；After flowing through adsorbent bed (16)
Unabsorbed gas phase arsenic and carrier gas enter tail gas absorption bottle (19), are discharged after absorbing liquid is washed.
Experiment flow is as described below: flow through the carrier gas of mass flowmenter (6) and preheated by oil bath, carry gas phase arsenic with react
Gas mixing forms air-flow containing arsenic, this air-flow containing arsenic passes through adsorbent bed (16) from bottom to top and reacts with adsorbent, do not inhaled
Attached gas phase arsenic and carrier gas is discharged after tail gas absorption bottle (19) are washed.
Specific embodiment is as described below:
Step 1: crystal reaction tube (17), gas phase arsenic generator (10) are connected and cover upper heat tracing pipe in designated position
(13), it is respectively placed in electric furnace (14) furnace chamber, oil bath pan (11), according to setting electric furnace (14), oil bath needed for experiment
Pot (11) and heat tracing pipe (13) temperature, is denoted as t respectively1、t2、t3, unit is DEG C；
Step 2: selection experiment is sorbent used, weighs its quality and is denoted as m1, adsorbent is evenly laid out in adsorbent bed
(16) on；
Step 3: it weighs crucible (8) quality and is denoted as m2, a certain amount of arsenic trioxide powder is added thereto, weighs sample
Product and crucible (8) gross mass are denoted as m3, then added sample quality is m3-m2, unit g；
Step 4: 5%HNO is prepared3/ 10%H2O2Solution measures the 100mL solution respectively and pours into two absorption bottles, adopts
Two absorption bottles are connected with hose；
Step 5: after electric furnace (14), oil bath pan (11) and heat tracing pipe (13) temperature are stablized, the earthenware of sample will be housed
Crucible (8) is placed in gas phase arsenic generator (10), and adsorbent bed (16) is placed in fixed position inside crystal reaction tube (17)；
Step 6: connection carrier gas is opened mass flowmenter (5,6), flow is denoted as F respectively1、F2, unit mL/min；
Step 7: being first shut off oil bath pan (11) after the reaction time needed for reaching, then successively close heat tracing pipe (13),
Electric furnace (14) after keeping carrier gas high-temperature blowing 15min, closes air valve and mass flowmenter (5,6).
Claims (6)
1. a kind of gas phase arsenic quantitatively occurs and adsorbent equipment, comprising: gas phase arsenic generating device, adsorbent equipment and tail gas absorption dress
It sets.Wherein: the gas phase arsenic generating device includes crucible (8), quartzy sieve plate (9), gas phase arsenic generator (10), oil bath pan
(11)；Gas adsorbing device includes crystal reaction tube (17), the adsorbent bed (16) being arranged in crystal reaction tube (17), small electrical
Heating furnace (14) and temperature controller (15)；Absorption plant includes tail gas absorption bottle (19).
2. gas phase arsenic as described in claim 1 quantitatively occurs and adsorbent equipment, it is characterised in that: oil bath heating is located at gas phase arsenic hair
Arsenic trioxide powder in raw device (10) is allowed to distillation and generates gas phase arsenic, and oil bath pan (11) is simultaneously to carrier gas and reaction gas
It is preheated, gas phase arsenic, which mixes under carrier gas carrying with reaction gas, to be flowed through adsorbent bed (16) and react with adsorbent, tail gas
In unadsorbed gas phase arsenic and carrier gas be discharged after tail gas absorption bottle (19) washing；It can using oil bath pan (11) heating method
The stabilization of temperature in experimentation is maintained, to quantitatively generate continual and steady air-flow containing arsenic；Reduce electric furnace (14)
Length reduces installation cost.
3. gas phase arsenic as described in claim 1 quantitatively occurs and adsorbent equipment, it is characterised in that: the gas phase arsenic generating device is logical
Cross heating sublimation arsenic trioxide powder and generate gas phase arsenic, and carried by carrier gas to adsorbent equipment, it is ensured that gas generant portion without
The influence of other factors；It is adjusted by the coupling to oil temperature and carrier gas flux, realizes the quantitative adjusting of arsenic content in air-flow；Pass through
Adjust heat tracing pipe (13) temperature, it is ensured that the gas for flowing through gas phase arsenic generator (10) outlet will not be condensed on tube wall；Gas phase arsenic
Generator is using " W " configuration and is placed in oil bath pan (11) heating, realizes the uniform mixing of air-flow, and carry out to inlet air flow
Preferable preheating.
4. gas phase arsenic as described in claim 1 quantitatively occurs and adsorbent equipment, it is characterised in that: the adsorbent equipment passes through adjusting
Electric furnace (14) temperature controls bed temperature, realizes the adsorption reaction under different temperatures；Adsorbent bed (16) can before and after experiment
To be removed, convenient for the pick-and-place and weighing of adsorbent, the precision of arsenic content in adsorbent is strengthened.
5. gas phase arsenic as described in claim 1 quantitatively occurs and adsorbent equipment, it is characterised in that: by adding absorbing liquid, both kept away
The harm for not absorbing gas to human health is exempted from, while can also be by arsenic content in measurement absorbing liquid, in conjunction with adsorbent institute
Arsenic-adsorbing amount is compared with sample losing quantity, it is ensured that total arsenic amount balance reduces experimental error.
6. gas phase arsenic as described in claim 1 quantitatively occurs and adsorbent equipment, it is characterised in that specific steps are as follows:
Step 1: crystal reaction tube (17), gas phase arsenic generator (10) are connected and cover upper heat tracing pipe (13) in designated position,
It is respectively placed in electric furnace (14) furnace chamber, oil bath pan (11), according to setting electric furnace (14), oil bath pan (11) needed for experiment
And heat tracing pipe (13) temperature, it is denoted as t respectively1、t2、t3, unit is DEG C；
Step 2: selection experiment is sorbent used, weighs its quality and is denoted as m1, adsorbent is evenly laid out on adsorbent bed (16)；
Step 3: it weighs crucible (8) quality and is denoted as m2, a certain amount of arsenic trioxide powder is added thereto, weighs sample and earthenware
Crucible (8) gross mass is denoted as m3, then added sample quality is m3-m2, unit g；
Step 4: 5%HNO is prepared3/ 10%H2O2Solution measures the 100mL solution respectively and pours into two absorption bottles, and use is soft
Pipe connects two absorption bottles；
Step 5: after electric furnace (14), oil bath pan (11) and heat tracing pipe (13) temperature are stablized, the crucible of sample will be housed
(8) it is placed in gas phase arsenic generator (10), adsorbent bed (16) is placed in fixed position inside crystal reaction tube (17)；
Step 6: connection carrier gas is opened mass flowmenter (5,6), flow is denoted as F respectively1、F2, unit mL/min；
Step 7: being first shut off oil bath pan (11) after the reaction time needed for reaching, and then successively closes heat tracing pipe (13), electricity adds
Hot stove (14) after keeping carrier gas high-temperature blowing 15min, closes air valve and mass flowmenter (5,6).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113233502A (en) * | 2021-05-08 | 2021-08-10 | 中南大学 | Device and method for stably generating and calibrating gaseous arsenic trioxide |
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| CN1062300A (en) * | 1990-10-30 | 1992-07-01 | 法国石油公司 | Allow gas by a kind of be the method that the material of matrix is removed arsenic with carrier and copper sulfide |
| US20110223088A1 (en) * | 2010-03-11 | 2011-09-15 | Ramsay Chang | Method and Apparatus for On-Site Production of Lime and Sorbents for Use in Removal of Gaseous Pollutants |
| CN107789975A (en) * | 2016-09-07 | 2018-03-13 | 中国科学院过程工程研究所 | A kind of dearsenicating method of high-temperature flue gas |
| CN207231874U (en) * | 2017-07-13 | 2018-04-13 | 中国神华能源股份有限公司 | Fixed combination equipment occurs for gas phase arsenic compound |
-
2019
- 2019-05-15 CN CN201910396350.7A patent/CN110465110A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1062300A (en) * | 1990-10-30 | 1992-07-01 | 法国石油公司 | Allow gas by a kind of be the method that the material of matrix is removed arsenic with carrier and copper sulfide |
| US20110223088A1 (en) * | 2010-03-11 | 2011-09-15 | Ramsay Chang | Method and Apparatus for On-Site Production of Lime and Sorbents for Use in Removal of Gaseous Pollutants |
| CN107789975A (en) * | 2016-09-07 | 2018-03-13 | 中国科学院过程工程研究所 | A kind of dearsenicating method of high-temperature flue gas |
| CN207231874U (en) * | 2017-07-13 | 2018-04-13 | 中国神华能源股份有限公司 | Fixed combination equipment occurs for gas phase arsenic compound |
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| Title |
|---|
| S.MAHULI, R.AGNIHOTRI, S.CHAUK, A.GHOSH-DASTIDAR, ANDL.-S.FAN: "Mechanism of Arsenic Sorption by Hydrated Lime", 《ENVIRONMENTAL SCIENCE & TECHNOLOGY》 * |
| 张月 等: "金属氧化物吸附剂干法脱除气相As2O3实验研究", 《燃料化学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113233502A (en) * | 2021-05-08 | 2021-08-10 | 中南大学 | Device and method for stably generating and calibrating gaseous arsenic trioxide |
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Application publication date: 20191119 |