CN102773013B - Method for purifying silicon tetrafluoride in industrial tail gas - Google Patents
Method for purifying silicon tetrafluoride in industrial tail gas Download PDFInfo
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- CN102773013B CN102773013B CN201210254127.7A CN201210254127A CN102773013B CN 102773013 B CN102773013 B CN 102773013B CN 201210254127 A CN201210254127 A CN 201210254127A CN 102773013 B CN102773013 B CN 102773013B
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- Prior art keywords
- tail gas
- ocratation
- catalyst
- potassium hydroxide
- industrial
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- 238000000034 method Methods 0.000 title claims abstract description 25
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 title abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims description 53
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 50
- 238000005406 washing Methods 0.000 claims description 19
- PYWXAAFODZDNNL-UHFFFAOYSA-N [Co].N#CC#N.[Ti] Chemical compound [Co].N#CC#N.[Ti] PYWXAAFODZDNNL-UHFFFAOYSA-N 0.000 claims description 18
- 238000006277 sulfonation reaction Methods 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 230000002779 inactivation Effects 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000006424 Flood reaction Methods 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 230000001172 regenerating effect Effects 0.000 claims description 2
- 230000000153 supplemental effect Effects 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims 1
- 239000003599 detergent Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 description 11
- 238000011069 regeneration method Methods 0.000 description 11
- 239000002440 industrial waste Substances 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000003245 coal Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 238000005352 clarification Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- MPPQGYCZBNURDG-UHFFFAOYSA-N 2-propionyl-6-dimethylaminonaphthalene Chemical compound C1=C(N(C)C)C=CC2=CC(C(=O)CC)=CC=C21 MPPQGYCZBNURDG-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 206010037423 Pulmonary oedema Diseases 0.000 description 1
- 208000010476 Respiratory Paralysis Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003444 anaesthetic effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 210000001508 eye Anatomy 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 201000004792 malaria Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 208000005333 pulmonary edema Diseases 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 210000003491 skin Anatomy 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a method for purifying silicon tetrafluoride in industrial tail gas. The method comprises the steps as follows: taking modified active carbon as a catalyst; and processing and purifying the industrial tail gas containing the silicon tetrafluoride under micro-aerobic conditions. The catalyst used in the method provided by the invention has the characteristics of low cost, high activity and good catalytic property; and the removal rate of the silicon tetrafluoride in the tail gas purified by the method is more than 95%.
Description
Technical field
The invention belongs to environmental protection technical field, be specifically related to the method for ocratation in a kind of purified industrial tail gas.
Background technology
Ocratation has another name called silicon fluoride, and molecular formula is SiF
4, be a kind of gas of colourless, poisonous, irritant stink.Easy deliquescence, the mist that can produce thick smoke in malaria, human body can cause headache, nauseating and anesthetic effect in various degree after sucking, to eye, skin, mucous membrane and respiratory tract have grievous injury and corrosiveness strong.High concentration inspirator can cause pneumonia, pulmonary edema, serious poisoningly causes respiratory paralysis and death.Ocratation is mainly present in the waste gas of industrial discharge, works for a long time and can cause serious harm to human body in this stimulation and suffocative stench environment.Always a large amount of industrial waste gases can discharge no matter how advanced its equipment is in now big and small chemical producer, wherein main waste gas has CO, NO
x, H
2s, HF, SiF
4deng, the correlative study that purifies ocratation due to industrial tail gas is less, and therefore removing ocratation has profound significance to the purification of industrial waste gas.
Publication number is 101134562 to disclose a kind of ocratation intermediate water that utilizes and absorb and be hydrolyzed, and makes the silicate fluoride solution of 10-40% after filtration, then makes prodan, although this WATER-WASHING METHOD is convenient and swift, is not suitable for high temperature preparation and removes.More than in industrial waste gas, general temperature reaches 500 degree, so WATER-WASHING METHOD is not suitable for using herein.
In the article " Thermodynamic modeling and gaseous pollution prediction of the yellow phosphorus production " that Zhonghua Wang etc. publishes in Industrial & Engineering Chemistry Research periodical the 50th volume 12194-12202 page, point out that ocratation content in yellow phosphoric tail gas reaches 0.04991g/m
3, be wantonly discharged in air and have very large harm, also there is no ripe removal method and approach at present.
For above problem, the present invention proposes the approach of removing ocratation in industrial waste gas, for China's tail gas clean-up proposes a feasible scheme.
Summary of the invention
The object of the present invention is to provide the method for ocratation in a kind of purified industrial tail gas, the method adopts modified activated carbon effectively to remove ocratation in tail gas, for China proposes a feasible scheme containing ocratation tail gas clean-up.
The present invention adopts following concrete technology flow process to realize the object of the invention:
1, catalyst preparation: large with 70 ℃ of deionized water wash ratio surface areas, the blank active carbon of space prosperity is to remove its surface dirt, active carbon is put into potassium hydroxide by solid-liquid mass ratio 1:5-10 and sulfonation titanium cyanogen cobalt mixed solution floods aging 24-36h, after filtration, with distilled water, wash 3-5 time, dry 12-24h at 90-120 ℃, then pass into nitrogen, roasting 6-10h at anoxic condition, 200-500 ℃, is purified catalyst used;
2. process for purifying flow process
(1) at fixed bed, add the catalyst preparing, sealing;
(2) heating fixation reaction bed passes into fixed reactor by the industrial tail gas that contains ocratation at 40-100 ℃, and reaction velocity is 100-300h
-1, and supplemental oxygen, the concentration of volume percent of oxygen in industrial tail gas is 0.2-2.0%, after adsorption treatment, tail gas is and purifies rear tail gas;
(3) after gas purification, chromatograph instrument detects silicon tetrafluoride gas concentration;
3, catalyst regeneration process flow process
After purifying, deactivated catalyzer with water steam washing 2-6 hour is then dried 12 hours, the catalyst after can regenerating at the temperature of 100-150 ℃.
In the present invention, potassium hydroxide and sulfonation titanium cyanogen cobalt mixed solution refer at 10%(W/V) potassium hydroxide solution in add sulfonation titanium cyanogen cobalt to prepare solution, wherein the mass ratio of potassium hydroxide and sulfonation titanium cyanogen cobalt is 1:0.1-5:0.1.
The advantage of the inventive method is: the active carbon after modification can be used in each factory the ocratation in industrial tail gas is effectively removed, and have the advantages that temperature is low, cost is low, activity is high, its plant investment operating cost is low, not limit by flue gas load and can produce hardly the accessory substances such as sewage, dirty acid.For the ocratation in the industrial waste gas of removal complicated ingredient, there is very considerable economic benefit, this catalyst is renewable and possess good catalytic performance, and environmental pollution is less, and technology is practical, tail gas after purifying by the inventive method, ocratation clearance is more than 95%.
The specific embodiment
Below by embodiment, the present invention is described in further detail, but protection domain of the present invention is not limited to described content.
Embodiment 1: the method for ocratation in this purified industrial tail gas, and concrete operations are as follows:
1,10.0g potassium hydroxide is dissolved in the aqueous solution of 100ml, then add under 1.0g sulfonation titanium cyanogen cobalt room temperature and be uniformly mixed, with 70 ℃ of deionized water washing diameters, it is 1.5mm coal mass active carbon, and 15g active carbon is inserted in potassium hydroxide and sulfonation titanium cyanogen cobalt mixed solution and flooded aging 24 hours, then by its filtration washing 5 times, at the temperature of 110 ℃, be dried 13 hours, put into afterwards Muffle furnace and pass into nitrogen, at anoxic condition, 200 ℃, roasting is 10 hours, is purified catalyst used;
2, modified catalyst is put into fixed bed, sealing, passes into the industrial waste gas that contains ocratation at 40 ℃, and filling into oxygen, to make the concentration of volume percent of oxygen in industrial tail gas be 0.5%, in tail gas, containing ocratation concentration, is wherein 79mg/m
3, reaction velocity is 300h
-1; Catalyst after 50 hours purify in gas ocratation concentration be 0.095mg/m
3below;
3, by the catalyzer with water steam washing after inactivation 2 hours, the catalyst at 110 ℃ after dry regeneration for 12 hours, the catalyst efficiency after regeneration still reaches 90%.
Embodiment 2: the method for ocratation in this purified industrial tail gas, and concrete operations are as follows:
1,20g potassium hydroxide is dissolved in the aqueous solution of 200ml, then add under 0.67g sulfonation titanium cyanogen cobalt room temperature and be uniformly mixed, the coal mass active carbon 10g that is 1.5mm with 70 ℃ of deionized waters washing diameters and insert 100ml potassium hydroxide and sulfonation titanium cyanogen cobalt mixed solution in flood aging 30 hours, then by its filtration washing 3 times, at the temperature of 90 ℃, do 24 hours, put into afterwards Muffle furnace and pass into nitrogen, at anoxic condition, 500 ℃, roasting is 6 hours, is purified catalyst used;
2, modified catalyst is put into fixed bed, sealing, passes into the industrial waste gas that contains ocratation at 50 ℃, and filling into oxygen, to make the concentration of volume percent of oxygen in industrial tail gas be 1%, in tail gas, containing ocratation concentration, is wherein 57.5mg/m
3, reaction velocity is 200h
-1; After adsorption cleaning, in gas, ocratation concentration is 0.089mg/m
3below, the clarification time can reach 60 hours;
3, by the catalyzer with water steam washing after inactivation 5 hours, the catalyst at 100 ℃ after dry regeneration for 12 hours, the catalyst efficiency after regeneration still reaches 95%.
Embodiment 3: the method for ocratation in this purified industrial tail gas, and concrete operations are as follows:
1,20g potassium hydroxide is dissolved in the aqueous solution of 200ml, then add under 0.4g sulfonation titanium cyanogen cobalt room temperature and be uniformly mixed, by the coal mass active carbon 40g that is 1.5mm with 70 ℃ of deionized waters washing diameters and insert 200ml potassium hydroxide and sulfonation titanium cyanogen cobalt mixed solution in flood aging 36 hours, then by its filtration washing 4 times, at the temperature of 120 ℃, do 12 hours, put into afterwards Muffle furnace and pass into nitrogen, at anoxic condition, 300 ℃, roasting is 7 hours, is purified catalyst used;
2, modified catalyst is put into fixed bed, sealing, passes into the industrial waste gas that contains ocratation at 60 ℃, and filling into oxygen, to make the concentration of volume percent of oxygen in industrial tail gas be 2%, in tail gas, containing ocratation concentration, is wherein 62.5mg/m
3, reaction velocity is 100h
-1; After adsorption cleaning, in gas, ocratation concentration is 0.07mg/m
3below, the clarification time can reach 60 hours;
3, by the catalyzer with water steam washing after inactivation 6 hours, the catalyst at 150 ℃ after dry regeneration for 12 hours, the catalyst efficiency after regeneration still reaches 98%.
Embodiment 4: the method for ocratation in this purified industrial tail gas, and concrete operations are as follows:
1,10g potassium hydroxide is dissolved in the aqueous solution of 100ml, then add under 0.5g sulfonation titanium cyanogen cobalt room temperature and be uniformly mixed, by the coal mass active carbon 13g that is 1.5mm with 70 ℃ of deionized waters washing diameters and insert 100ml potassium hydroxide and sulfonation titanium cyanogen cobalt mixed solution in flood aging 28 hours, then by its filtration washing 4 times, at the temperature of 100 ℃, do 18 hours, put into afterwards Muffle furnace and pass into nitrogen, at anoxic condition, 400 ℃, roasting is 8 hours, is purified catalyst used;
2, modified catalyst is put into fixed bed, sealing, passes into the industrial waste gas that contains ocratation at 100 ℃, and filling into oxygen, to make the concentration of volume percent of oxygen in industrial tail gas be 0.2%, in tail gas, containing ocratation concentration, is wherein 68.5mg/m
3, reaction velocity is 150h
-1; After adsorption cleaning, in gas, ocratation concentration is 0.071mg/m
3below, the clarification time can reach 53 hours;
3, by the catalyzer with water steam washing after inactivation 4 hours, the catalyst at 120 ℃ after dry regeneration for 12 hours, the catalyst efficiency after regeneration still reaches 96%.
Embodiment 5: the method for ocratation in this purified industrial tail gas, and concrete operations are as follows:
1,10g potassium hydroxide is dissolved in the aqueous solution of 100ml, then add under 0.25g sulfonation titanium cyanogen cobalt room temperature and be uniformly mixed, by the coal mass active carbon 17g that is 1.5mm with 70 ℃ of deionized waters washing diameters and insert 100ml potassium hydroxide and sulfonation titanium cyanogen cobalt mixed solution in flood aging 25 hours, then by its filtration washing 3 times, at the temperature of 115 ℃, do 14 hours, put into afterwards Muffle furnace and pass into nitrogen, at anoxic condition, 250 ℃, roasting is 9 hours, is purified catalyst used;
2, modified catalyst is put into fixed bed, sealing, passes into the industrial waste gas that contains ocratation at 70 ℃, and filling into oxygen, to make the concentration of volume percent of oxygen in industrial tail gas be 1.5%, in tail gas, containing ocratation concentration, is wherein 70.5mg/m
3, reaction velocity is 250h
-1; After adsorption cleaning, in gas, ocratation concentration is 0.073mg/m
3below, the clarification time can reach 61 hours;
3, by the catalyzer with water steam washing after inactivation 3 hours, the catalyst at 130 ℃ after dry regeneration for 12 hours, the catalyst efficiency after regeneration still reaches 93%.
Claims (1)
1. a method for ocratation in purified industrial tail gas, is characterized in that carrying out as follows:
(1) with after 70 ℃ of deionized water detergent active charcoal dusts, active carbon is put into potassium hydroxide by solid-to-liquid ratio 1:5-10 and sulfonation titanium cyanogen cobalt mixed solution floods aging 24-36h, after filtration, with distilled water, wash 3-5 time, dry 12-24h at 90-120 ℃, then pass into nitrogen, roasting 6-10h at anoxic condition, 200-500 ℃, is purified catalyst used;
(2) modified catalyst is put into fixed bed, sealing passes into the industrial tail gas that contains ocratation at heating condition 40-100 ℃, and reaction velocity is 100-300h
-1, and supplemental oxygen, the concentration of volume percent of oxygen in industrial tail gas is 0.2-2%, after adsorption treatment, tail gas is and purifies rear tail gas;
(3) inactivation rear catalyst is with after steam washing 2-6h, and at 100-150 ℃, dry 12h, obtains the rear catalyst of regenerating, and is cycled to used in purified industrial ocratation tail gas;
The mixed solution of wherein said potassium hydroxide and sulfonation titanium cyanogen cobalt refers to the solution that adds sulfonation titanium cyanogen cobalt and prepare in 10% potassium hydroxide solution, and wherein the mass ratio of potassium hydroxide and sulfonation titanium cyanogen cobalt is 1:0.1-5:0.1.
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CN201210254127.7A CN102773013B (en) | 2012-07-23 | 2012-07-23 | Method for purifying silicon tetrafluoride in industrial tail gas |
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CN201210254127.7A CN102773013B (en) | 2012-07-23 | 2012-07-23 | Method for purifying silicon tetrafluoride in industrial tail gas |
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CN102773013B true CN102773013B (en) | 2014-11-05 |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1286644A (en) * | 1998-09-22 | 2001-03-07 | 日本派欧尼股份株式会社 | Purifying agent and purification method for halogen-contg. exhaust gas |
CN1398658A (en) * | 2002-04-26 | 2003-02-26 | 昆明理工大学 | Catalytic yellow phosphorus tail gas oxidizing and purifying method in fixed bed |
CN101590408A (en) * | 2008-05-27 | 2009-12-02 | 北京三聚环保新材料股份有限公司 | Thiols conversion catalyst and preparation method thereof |
US7641867B2 (en) * | 1997-11-14 | 2010-01-05 | Hitachi, Ltd. | Apparatus for processing perfluorocarbon |
-
2012
- 2012-07-23 CN CN201210254127.7A patent/CN102773013B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7641867B2 (en) * | 1997-11-14 | 2010-01-05 | Hitachi, Ltd. | Apparatus for processing perfluorocarbon |
CN1286644A (en) * | 1998-09-22 | 2001-03-07 | 日本派欧尼股份株式会社 | Purifying agent and purification method for halogen-contg. exhaust gas |
CN1398658A (en) * | 2002-04-26 | 2003-02-26 | 昆明理工大学 | Catalytic yellow phosphorus tail gas oxidizing and purifying method in fixed bed |
CN101590408A (en) * | 2008-05-27 | 2009-12-02 | 北京三聚环保新材料股份有限公司 | Thiols conversion catalyst and preparation method thereof |
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