CN1483503A - Method for recovering aromatic hydrocarbon in tail gas of oxydol production apparatus - Google Patents
Method for recovering aromatic hydrocarbon in tail gas of oxydol production apparatus Download PDFInfo
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- CN1483503A CN1483503A CNA021354898A CN02135489A CN1483503A CN 1483503 A CN1483503 A CN 1483503A CN A021354898 A CNA021354898 A CN A021354898A CN 02135489 A CN02135489 A CN 02135489A CN 1483503 A CN1483503 A CN 1483503A
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- aromatic hydrocarbons
- active carbon
- tail gas
- aromatic hydrocarbon
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract
The method for purifying and recovering aromatic hydrocarbon in the tail gas of oxydol production equipment adopts the pretreated active carbon catalyst as adsorption agent to remove aromatic hydrocarbon and recover and reuse it. Its adsorption condition is as follows: tail gas pressure is 0.2-2 MPa, temp. is 0-40 deg.C, space velocity is 100-2000 h(-1), and the inlet aromatic hydrocarbon content is less han or equal to 1000 ppm generally; then it uses the superheated stream or N2 to heat at 120 deg.C-400 deg.C to make desorption, and make cooling treatment so as to recover aromatic hydrocarbon.
Description
Technical field
The present invention relates to the purification-recovery method of aromatic hydrocarbons in the tail gas of oxydol production apparatus, more specifically, the present invention relates to C in a kind of tail gas of oxydol production apparatus
8-C
11Purification-the recovery method of aromatic hydrocarbons.
Background technology
The purification of aromatic hydrocarbons-recovery requirement is relevant with the consumption reduction of environmental protection and device in the oxydol production apparatus emptying end gas.Domestic oxydol production apparatus great majority have adopted subcooled method to reclaim to the aromatic hydrocarbons in the emptying end gas.But the content of aromatic hydrocarbons is still very high in the tail gas of cooling back (5-10 ℃), about about 3000-7000ppm, is higher than 10000ppm sometimes.This does not only reach environmental requirement, makes the loss of aromatic hydrocarbons high yet, causes waste, has increased production cost.(for example " Chemical Engineering " magazine was rolled up " hydrogen peroxide oxidation tail gas bi-level treatment art designs " disclosed method of the 6th phase P47-50 in 1999 27 although some producer has also increased charcoal treatment, it is the cellular active carbon adsorption aromatic hydrocarbons of TF type that adopts general Shoes Factory and Paint Factory's exhaust-gas treatment), but effect is undesirable.Can remove the aromatic hydrocarbons in the tail gas efficiently, the protection environment again can recycling aromatic hydrocarbons, reduces the wastage, and has not yet to see the method for effective practicality.
Summary of the invention
Purification-the recovery method of aromatic hydrocarbons in the tail gas of oxydol production apparatus of the present invention is to adopt through pretreated activated-carbon catalyst to remove aromatic hydrocarbons and in addition recycling in the tail gas as adsorbent.As the active carbon (preferred size is the active carbon of Φ 3-7mm) of adsorbent, must can meet the demands through preliminary treatment.Described preliminary treatment is to adopt one of following method to handle active carbon:
(1) with concentration be 0.1～1.0M diluted acid to active carbon carry out acid pickling, acid is boiled or pickling, carries out drying more according to a conventional method, then at N
2Roasting under the atmosphere (preferred 150 ℃～450 ℃ of sintering temperature), wherein diluted acid can adopt HCl, HNO
3, H
2SO
4Or its mixture;
(2) be that the alkaline substance solution of 0.1～1.0M carries out alkali steeping, soda boiling or alkali cleaning to active carbon with concentration, carry out drying more according to a conventional method, then at N
2Roasting under the atmosphere (preferred 150 ℃～450 ℃ of sintering temperature), wherein alkaline matter can adopt NaOH, KOH, Mg (OH)
2, Na
2CO
3, K
2CO
3Or its mixture;
(3) with concentration be the salt solution impregnation active carbon of 0.1～2.0M, carry out drying more according to a conventional method, then at N
2Roasting under the atmosphere (preferred 150 ℃～450 ℃ of sintering temperature), wherein salt can adopt Cu (NO
3)
2, Zn (NO
3)
2, Co (NO
3)
2, Ni (NO
3)
2, Ag (NO
3)
2Deng or its mixture;
(4) with above-mentioned (1) and/or (2) active carbon is handled, used above-mentioned (3) to handle again.
More preferably 200 ℃～300 ℃ of above-mentioned sintering temperatures.
Liang difference as required, with the pretreated acticarbon of the present invention of above-mentioned process, pack in the container of certain volume, by following condition the aromatic hydrocarbons in the tail gas of oxydol production apparatus is adsorbed-reclaims, adsorption conditions is: tail gas pressure 0.2-2MPa, temperature 0-40 ℃, air speed 100-2000h
-1, the inlet arene content is general≤10000ppm; Aromatic recovery (or adsorbent reactivation) adopts general known method, and the preferred regenerating medium that adopts is superheated steam or nitrogen, and its temperature is 120 ℃～400 ℃, chilling temperature≤10 ℃.
The present invention is active high to aromatic hydrocarbons adsorbing and removing in the tail gas of oxydol production apparatus, and adsorbance is big, the aromatic recovery rate height, and technology is simple, and easy operating is suitable for industrialization and adopts, both can satisfy environmental requirement, and can reduce the consumption of aromatic hydrocarbons again, improve the input/output ratio of device.
The specific embodiment
Below by Comparative Examples and embodiment technology of the present invention is given to illustrate further.Comparative Examples one:
Selecting granularity for use is the common active carbon of Φ 3 * 5mm, does not do preliminary treatment, and getting the 1000ml volume of packing into is in the reactor of 1000ml, and adsorption conditions is: tail gas pressure 0.2MPa, 35 ℃ of temperature, air speed 1000h
-1, inlet arene content 4400ppm, 24h outlet aromatic hydrocarbons average content is 160ppm.
Above-mentioned sample of sorbent fully is adsorbed to no longer weightening finish, and this moment, adsorption rate was 22.04%.Reactor is fed superheated steam more than 140 ℃, and outlet connects the coiled water cooling heat exchanger, uses separatory funnel to separate the grease in the liquid of cooling, and the aromatic hydrocarbons that records recovery accounts for 22.8% of total augment weight.
Embodiment one:
Selecting granularity for use is the common active carbon of Φ 3 * 5mm, uses 1MHNO
3Flood 12h and handle, oven dry then, logical N
2Under 200 ℃, carry out roasting.Getting the 1000ml volume of packing into is in the reactor of 1000ml, and adsorption conditions is with Comparative Examples one, inlet arene content 5000ppm, and aromatic hydrocarbons outlet content is 210ppm.
Above-mentioned sample of sorbent fully is adsorbed to no longer weightening finish, and this moment, adsorption rate was 34.2%, took off sample, and reactor is fed 180 ℃ of N
2, outlet connects the coiled water cooling heat exchanger, and the aromatic hydrocarbons that cools off is reclaimed, and the aromatic hydrocarbons that records recovery accounts for 79.7% of total augment weight.Repeat absorption, regenerative process, the secondary recovery rate is 94.6%.
Embodiment two:
It is some to get embodiment one handled active carbon, with the Zn (NO of equal-volume 0.2M
3)
2N is dried, led to dipping 12h then
2Carry out roasting under 200 ℃, adsorption conditions is with embodiment one, inlet arene content 5600ppm, reactor outlet arene content＜100ppm.
Above-mentioned sample of sorbent fully is adsorbed to no longer weightening finish, and this moment, adsorption rate was 38.5%, took off sample, and reactor is fed 180 ℃ of N
2, outlet connects the coiled water cooling heat exchanger, and the aromatic hydrocarbons that cools off is reclaimed, and the aromatic hydrocarbons that records recovery accounts for 76.1% of total augment weight.Repeat absorption, regenerative process, the secondary recovery rate is 104.9%.
Embodiment three:
Selecting granularity for use is the common active carbon of Φ 3 * 5mm, uses 0.2MNaOH to flood 12h and handles, oven dry then, logical N
2Under 200 ℃, carry out roasting.Getting the 600ml volume of packing into is in the reactor of 1000ml, and adsorption conditions is with embodiment one, inlet arene content 4000ppm, aromatic hydrocarbons outlet content＜100ppm.
Above-mentioned sample of sorbent fully is adsorbed to no longer weightening finish, and this moment, adsorption rate was 25.7%, took off sample, and reactor is fed 180 ℃ of N
2, outlet connects the coiled water cooling heat exchanger, and the aromatic hydrocarbons that cools off is reclaimed, and the aromatic hydrocarbons that records recovery accounts for 70.9% of total augment weight.Repeat absorption, regenerative process, the secondary recovery rate is 96.5%.
Embodiment four:
Selecting granularity for use is the common active carbon of Φ 3 * 5mm, at first uses 1MHNO
3N is dried, led to dipping 12h
2Under 200 ℃, carry out roasting; Flood 12h with 0.2MNaOH again, dry, lead to N
2Under 200 ℃, carry out roasting; The above active carbon of handling of learning from else's experience was some, and then with the Zn (NO of equal-volume 0.2M
3)
2N is dried, led to dipping 12h
2Carry out roasting under 200 ℃, adsorption conditions is with embodiment one, inlet arene content 5000ppm, reactor outlet arene content＜100ppm.
Above-mentioned sample of sorbent fully is adsorbed to no longer weightening finish, and this moment, adsorption rate was 35.2%, took off sample, and reactor is fed 180 ℃ of N
2, outlet connects the coiled water cooling heat exchanger, and the aromatic hydrocarbons that cools off is reclaimed, and the aromatic hydrocarbons that records recovery accounts for 84.8% of total augment weight.Repeat absorption, regenerative process, the secondary recovery rate is 96.6%.
Claims (10)
1. purification-the recovery method of aromatic hydrocarbons in the tail gas of oxydol production apparatus is characterized in that adopting through pretreated activated-carbon catalyst as adsorbent aromatic hydrocarbons being removed and reclaiming.
2. by the described method of claim 1, it is characterized in that adsorption conditions is: tail gas pressure 0.2-2.0MPa, temperature 0-40 ℃, air speed 100-2000h
-1
3. according to claim 1 or 2 described methods, it is characterized in that described preliminary treatment is to adopt one of following method to handle active carbon:
(1) with concentration be 0.1～1.0M diluted acid to active carbon carry out acid pickling, acid is boiled or pickling, carries out drying more according to a conventional method, then at N
2Roasting under the atmosphere, wherein diluted acid can adopt HCl, HNO
3, H
2SO
4Or its mixture;
(2) be that the alkaline substance solution of 0.1～1.0M carries out alkali steeping, soda boiling or alkali cleaning to active carbon with concentration, carry out drying more according to a conventional method, then at N
2Roasting under the atmosphere, wherein alkaline matter can adopt NaOH, KOH, Mg (OH)
2, Na
2CO
3, K
2CO
3Or its mixture;
(3) with concentration be the salt solution impregnation active carbon of 0.1～2.0M, carry out drying more according to a conventional method, then at N
2Roasting under the atmosphere, wherein salt can adopt Cu (NO
3)
2, Zn (NO
3)
2, Co (NO
3)
2, Ni (NO
3)
2, Ag (NO
3)
2Deng or its mixture;
(4) with above-mentioned (1) and/or (2) active carbon is handled, used above-mentioned (3) to handle again.
4. by the described purification-recovery method of claim 3, wherein sintering temperature is 150 ℃～450 ℃.
5. by the described purification-recovery method of claim 3, wherein sintering temperature is 200 ℃～300 ℃.
6. by the described method of claim 1, wherein aromatic recovery or catalyst regeneration condition are: regenerating medium uses steam or nitrogen, and temperature is 120 ℃～400 ℃.
7. by claim 1 or 2 described methods, wherein the granularity of active carbon is Φ 3-7mm.
8. by the described method of claim 3, wherein the granularity of active carbon is Φ 3-7mm.
9. by claim 1 or 2 described methods, wherein said aromatic hydrocarbons is that carbon number is C
8-C
11Aromatic hydrocarbons.
10. by the described method of claim 5, wherein said aromatic hydrocarbons is that carbon number is C
8-C
11Aromatic hydrocarbons.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02135489 CN1200758C (en) | 2002-09-20 | 2002-09-20 | Method for recovering aromatic hydrocarbon in tail gas of oxydol production apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02135489 CN1200758C (en) | 2002-09-20 | 2002-09-20 | Method for recovering aromatic hydrocarbon in tail gas of oxydol production apparatus |
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| Publication Number | Publication Date |
|---|---|
| CN1483503A true CN1483503A (en) | 2004-03-24 |
| CN1200758C CN1200758C (en) | 2005-05-11 |
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ID=34146172
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02135489 Expired - Fee Related CN1200758C (en) | 2002-09-20 | 2002-09-20 | Method for recovering aromatic hydrocarbon in tail gas of oxydol production apparatus |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101890271A (en) * | 2010-07-21 | 2010-11-24 | 东营华泰纸业化工有限公司 | Method for improving gas recovery rate of aromatic hydrocarbon in production of hydrogen peroxide |
| CN102008862A (en) * | 2010-09-20 | 2011-04-13 | 上海安赐机械设备有限公司 | Recovery unit and recovery method for aromatic hydrocarbon in tail gas in hydrogen peroxide production process |
| CN103372357A (en) * | 2012-04-23 | 2013-10-30 | 怀化市双阳林化有限公司 | Method and device for processing oxidized tail gas of anthraquinone process-based hydrogen peroxide production |
| CN108815987A (en) * | 2018-07-24 | 2018-11-16 | 冯日洪 | Hydrogen peroxide oxidation exhaust treatment system and processing method |
| CN109420475A (en) * | 2017-08-23 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of adsorbent and preparation method thereof for adsorbing aromatic hydrocarbon substance |
-
2002
- 2002-09-20 CN CN 02135489 patent/CN1200758C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101890271A (en) * | 2010-07-21 | 2010-11-24 | 东营华泰纸业化工有限公司 | Method for improving gas recovery rate of aromatic hydrocarbon in production of hydrogen peroxide |
| CN102008862A (en) * | 2010-09-20 | 2011-04-13 | 上海安赐机械设备有限公司 | Recovery unit and recovery method for aromatic hydrocarbon in tail gas in hydrogen peroxide production process |
| CN102008862B (en) * | 2010-09-20 | 2012-10-10 | 上海安赐机械设备有限公司 | Recovery method for aromatic hydrocarbon in tail gas in hydrogen peroxide production process |
| CN103372357A (en) * | 2012-04-23 | 2013-10-30 | 怀化市双阳林化有限公司 | Method and device for processing oxidized tail gas of anthraquinone process-based hydrogen peroxide production |
| CN109420475A (en) * | 2017-08-23 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of adsorbent and preparation method thereof for adsorbing aromatic hydrocarbon substance |
| CN108815987A (en) * | 2018-07-24 | 2018-11-16 | 冯日洪 | Hydrogen peroxide oxidation exhaust treatment system and processing method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1200758C (en) | 2005-05-11 |
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Owner name: CHINA PETROLEUM & CHEMICAL CORPORATION Free format text: FORMER OWNER: QILU PETROCHEMICAL GROUP CO., CHINA PETROCHEMICAL CORP. Effective date: 20071228 |
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Effective date of registration: 20071228 Address after: Linzi Zibo District, Shandong province Sinopec Qilu Branch of science and technology Patentee after: Sinopec Corp. Address before: Linzi District of Shandong city of Zibo province Huan Road No. 15 Patentee before: Qilu Petrochemical Co., China Petrochemical Group Corp. |
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Granted publication date: 20050511 Termination date: 20130920 |