CN109420475A - A kind of adsorbent and preparation method thereof for adsorbing aromatic hydrocarbon substance - Google Patents
A kind of adsorbent and preparation method thereof for adsorbing aromatic hydrocarbon substance Download PDFInfo
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- CN109420475A CN109420475A CN201710727981.3A CN201710727981A CN109420475A CN 109420475 A CN109420475 A CN 109420475A CN 201710727981 A CN201710727981 A CN 201710727981A CN 109420475 A CN109420475 A CN 109420475A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0222—Compounds of Mn, Re
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/25—Coated, impregnated or composite adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7027—Aromatic hydrocarbons
Abstract
The present invention provides a kind of preparation methods of aromatic hydrocarbon substance high-efficiency adsorbent, can protect environment and recycle in tail gas using substance.Detailed process is to prepare aromatic hydrocarbon substance adsorbent first: preparing the oxyacid solns such as nitric acid, phosphoric acid, formic acid, acetic acid.Above-mentioned solution is active carbon treatment fluid, after processing, is filtered, washed, dries, loads in salting liquid containing manganese Metal, and adsorbent is made after filtering, roasting.Adsorbent is applied to aromatic hydrocarbon substance vent gas treatment, and recycling can be desorbed after absorption.
Description
Technical field
The present invention is a kind of adsorbent and preparation method thereof for adsorbing aromatic hydrocarbon substance.
Background technique
Aromatic hydrocarbons is the substances such as the general name of the hydrocarbon containing benzene ring structure, including benzene, toluene, biphenyl.Aromatic hydrocarbons object
Matter is the important source material in Chemical Manufacture, and aromatic hydrocarbon substance has toxicity mostly, partially has carcinogenicity, sucks or contact and is highly concentrated
Degree aromatic hydrocarbon substance can cause harm to the human body.As society increasingly pays close attention to environmental issue, country is more next to environmental protection supervision
It is stringenter, handle aromatic hydrocarbon substance pollution problem well, can qualified discharge be the key that ensure process units stable operation it
One.
Combustion method is common processing aromatic hydrocarbon substance method, and method and process process is simple, high treating effect, is easy real
Existing 100% purification, but there is the disadvantages of energy consumption is high, equipment investment is high in it, and practicability is subject to certain restrictions.
Absorption method is to handle the purification method of aromatic hydrocarbon substance by physical absorption or chemisorption with adsorbent, common
Adsorption method includes active carbon adsorption, metal oxide absorption method, temp.-change adsorptive process etc..Activated carbon adsorption is typically to adsorb
Method, but activated carbon adsorption aromatic hydrocarbon substance is used merely, mainly physical absorption is worked, and adsorption effect is poor, adsorption capacity
It is small.The processing of the means such as chemical modification is carried out to acticarbon, adsorbent is prepared, makes it in the process of absorption aromatic hydrocarbon substance
Middle generation chemisorption can effectively improve adsorbent absorption property, increase adsorption capacity.
US patent 5182088 is active component, then is added the promotors such as AgO, HgO using copper, zinc oxide, with co-precipitation
The adsorbent of method preparation has been obviously improved adsorption capacity, but due to being added to noble metal or high pollution heavy metal, certainly will increase
Preparation cost and subsequent treatment cost.
Aromatic hydrocarbon substance high-efficiency adsorbent is developed, different occasion aromatic hydrocarbon substances can be suitable for and handled, to protection ring
Border has positive effect.
Summary of the invention
Aromatic hydrocarbon substance cause environmental pollution there are aiming at the problem that, the present invention provides a kind of aromatic hydrocarbon substances efficiently to inhale
Attached dose and preparation method thereof, GB31571-215 petro chemical industry pollutant emission standard can be met, while recycling can benefit
Use substance.
Main technical schemes of the invention: one kind is for adsorbing aromatic hydrocarbon substance adsorbent, it is characterized in that adsorbent is selected
Active carbon is carrier, specific surface area >=680m2·g-1, granularity is 5-8 mesh, Kong Rongwei 0.27-0.35cm3·g-1, aperture is micro-
Hole 1.2-1.7nm, surface manganese content >=2.0%, section manganese content >=1.0%.
The present invention is used for the adsorbent of aromatic hydrocarbon substance, aromatic hydrocarbon substance gas-dynamic adsorbance 300-400mg/g, liquid
Adsorbance 500-700mg/g can apply it to aromatic hydrocarbon substance vent gas treatment and liquid leakage processing.
The present invention for aromatic hydrocarbon substance adsorbent preparation method, it is characterized in that prepare adsorbent use active carbon for
Carrier first prepares the oxyacid solns such as nitric acid, phosphoric acid, formic acid, acetic acid.It filters, is washed with deionized water after acid-washed active carbon
To certain pH value, active carbon after being dried in vacuo to handle.Potassium permanganate, sodium permanganate, manganese nitrate, manganese acetate etc. are prepared containing manganese gold
Belong to salting liquid, by active carbon after processing by above-mentioned solution loadings, after filtering, roasts and adsorbent is made.
Of the invention is used in including following occasion: (1) aromatic hydrocarbon substance tail gas adsorption；(2) at aromatic hydrocarbon substance liquid leakage
Reason.
The preparation method of the aromatic hydrocarbon substance adsorbent, used solution are nitric acid, phosphoric acid, formic acid, acetic acid etc.
Oxyacid soln, concentration 0.5-5mol/L.Above-mentioned solution is active carbon treatment fluid, processing mode are as follows: 1. pickling solution passes through
The fluidization wash of active carbon bed；Or 2. active carbon is placed in batch can, the agitator treating in acid solution；Or it 3. stands.Knot
It being filtered after beam, deionized water is washed to pH value 6-7, dry 6-12h, and 60-120 DEG C of drying temperature, active carbon after must handling.
The condition of processing mode 1. are as follows: treatment fluid liquid hourly space velocity (LHSV) 30-60h-1, 20-40 DEG C of temperature, time 0.5-1h；Processing
The condition of mode 2. are as follows: treatment fluid is 3:1-6:1, mixing speed 200-400r/min, temperature 20-50 with active carbon volume ratio
DEG C, time 2-4h；The condition of processing mode 3. are as follows: treatment fluid and active carbon volume ratio are 1.5:1-2:1,30-60 DEG C of temperature, when
Between 8-12h.
The preparation method of the aromatic hydrocarbon substance adsorbent, used maceration extract are potassium permanganate, sodium permanganate, nitre
The salting liquids containing manganese Metal such as sour manganese, manganese acetate, manganese content 0.1-0.4mol/L bear active carbon after processing by above-mentioned solution
It carries, mode of loading are as follows: 1. load fluidization wash of the liquid by active carbon bed；Or 2. active carbon is placed in batch can, in negative
Agitator treating in carrier fluid；Or it 3. stands.After filter.2-6h is roasted after load under the conditions of 300-600 DEG C, is made
Aromatic hydrocarbon substance adsorbent.
The condition of mode of loading 1. are as follows: load liquid liquid hourly space velocity (LHSV) 10-30h-1, 20-40 DEG C of temperature, time 1-2h；Load side
The condition of formula 2. are as follows: loaded liquid is long-pending and active carbon volume ratio is 3:1-6:1, mixing speed 200-300r/min, temperature 20-40
DEG C, time 4-8h；The condition of mode of loading 3. are as follows: it is 2:1-4:1 with active carbon volume ratio that loaded liquid is long-pending, 20-40 DEG C of temperature,
Time 10-16h.
The aromatic hydrocarbon substance adsorbent aromatic hydrocarbon substance tail gas adsorption of preparation, tail gas air speed 100-200h-1, normal temperature and pressure,
Steam or roasting desorption.
The method of the present invention realizes the efficient absorption of aromatic hydrocarbon substance, makes to protect environment, while having recycled using object
Matter.
Specific embodiment
The method of the present invention is described in detail below with reference to embodiment.
Embodiment 1
0.5mol/L nitric acid solution is prepared, passes through the fluidization wash formal layout active carbon of active carbon bed using pickling solution,
Treatment fluid liquid hourly space velocity (LHSV) 30h-1, 40 DEG C of temperature, time 1h.After filter, be washed with deionized to pH be 6, in 60 DEG C of items
Dry 12h, obtains nitric acid and washes rear active carbon under part.0.1mol/L liquor potassic permanganate is prepared, nitric acid is washed into rear active carbon and is placed in material
In tank, agitator treating mode is loaded in liquor potassic permanganate, and load liquid and active carbon volume ratio are 3:1, mixing speed 200r/
Min, 25 DEG C of temperature, time 4h.After filter, in 300 DEG C of roasting 6h, aromatic hydrocarbon substance adsorbent is made, sample characterization is such as
Shown in following table:
10wt/a chlorobenzene production device, tail gas enter 2000mg/m containing chlorobenzene before absorbing unit3, exhaust flow 1000m3/ h inhales
Coupon member adsorbent inventory 5t, empties after adsorbing, and wherein chlorobenzene is less than 40mg/m3.After operating time 1500h, close to row
Put standard limited value, 2h are desorbed using 150 DEG C of steam in adsorbent after use desorption, after nitrogen purge 2h.It repeats to be desorbed secondary
Number see the table below with operating time, replace adsorbent after desorption 4 times.
| Number is desorbed | Operating time h | Chlorobenzene content mg/m3 |
| 0 | 1500 | 48.1 |
| 1 | 1200 | 47.6 |
| 2 | 700 | 48.3 |
| 3 | 300 | 49.2 |
| 4 | 160 | 48.6 |
Embodiment 2
5mol/L acetic acid solution is prepared, is placed in batch can using active carbon, the agitator treating formal layout active carbon in acid solution.Place
Managing liquid and active carbon volume ratio is 6:1, stirring rate 300r/min, 30 DEG C of temperature, time 2h.After filter, use deionization
Water washing is 7 to pH, and dry 6h, obtains acetic acid and wash rear active carbon under the conditions of 120 DEG C.0.4mol/L manganese nitrate solution is prepared, it is molten
Liquid and active carbon volume ratio are 2:1, and nitric acid is washed rear active carbon and is loaded by standing form, 40 DEG C of dwell temperature, time 16h.
After filter, in 600 DEG C of roasting 2h, aromatic hydrocarbon substance adsorbent is made, sample characterization is as shown in the table:
5wt/a neighbour's chlorine para-aminotoluene process units, tail gas enter 800mg/m containing toluene before absorbing unit3, exhaust flow
600m3/ h, absorbing unit loadings 1t, empties after adsorbing, wherein toluene=6.1mg/m3.After operating time 3500h, benzene=
14.7mg/m3, close to limited value of discharge standard, 2h are desorbed using 150 DEG C of steam in adsorbent after use desorption, after nitrogen blow
Sweep 2h.Repeat desorption number see the table below with operating time, replace adsorbent after desorption 4 times.
| Number is desorbed | Operating time h | Toluene level mg/m3 |
| 0 | 3500 | 14.7 |
| 1 | 2200 | 13.9 |
| 2 | 1500 | 14.3 |
| 3 | 800 | 13.8 |
| 4 | 300 | 14.1 |
Embodiment 3
1mol/L phosphate aqueous solution is prepared, by active carbon by standing formal layout.Treatment conditions are phosphoric acid solution volume and work
Property charcoal volume ratio be 2:1,40 DEG C of temperature, time 12h.After filter, be washed with deionized to pH be 6.5, in 60 DEG C of items
Dry 9h, obtains phosphoric acid and washes rear active carbon under part.0.2mol/L sodium permanganate solution is prepared, sodium permanganate solution passes through active-carbon bed
The fluidization wash form load of layer, condition are solution liquid hourly space velocity (LHSV) 20h-1, 20 DEG C of temperature, time 1h.After filtering in 400
DEG C roasting 4h, is made aromatic hydrocarbon substance adsorbent, sample characterization is as shown in the table:
6wt/a producing cyclohexane by benzene hydrogenation process units, tail gas enter 600mg/m containing benzene before absorbing unit3Exhaust flow 500m3/
H, absorbing unit loadings 2t, empties after adsorbing, wherein benzene=2mg/m3.After operating time 1800h, benzene=5.3mg/m3, connect
2h are desorbed using 150 DEG C of steam in nearly limited value of discharge standard, the adsorbent desorption after use, after nitrogen purge 2h.It repeats de-
Attached number see the table below with operating time, replace adsorbent after desorption 4 times.
| Number is desorbed | Operating time h | Benzene content mg/m3 |
| 0 | 1800 | 3.3 |
| 1 | 1500 | 3.9 |
| 2 | 1100 | 3.8 |
| 3 | 600 | 3.7 |
| 4 | 200 | 3.6 |
Embodiment 4
1mol/L formic acid solution is prepared, passes through the fluidization wash formal layout active carbon of active carbon bed, place using pickling solution
Manage liquid liquid hourly space velocity (LHSV) 40h-1, temperature 50 C, time 2h.After filter, be washed with deionized to pH be 6.2, in 60 DEG C of items
Dry 12h, obtains nitric acid and washes rear active carbon under part.0.1mol/L liquor potassic permanganate is prepared, formic acid is washed into rear active carbon and is placed in material
In tank, agitator treating mode is loaded in liquor potassic permanganate, and load liquid and active carbon volume ratio are 3:1, mixing speed 200r/
Min, 25 DEG C of temperature, time 4h.After filter, in 300 DEG C of roasting 6h, aromatic hydrocarbon substance adsorbent is made, sample characterization is such as
Shown in following table:
20wt/a toluene process units, tail gas enter 1000mg/m containing toluene before absorbing unit3, exhaust flow 2000m3/ h inhales
Coupon member adsorbent inventory 10t, empties after adsorbing, and wherein toluene is less than 7.0mg/m3.After operating time 2000h, approach
2h are desorbed using 150 DEG C of steam in limited value of discharge standard, the adsorbent desorption after use, after nitrogen purge 2h.It repeats to be desorbed
Number see the table below with operating time, replace adsorbent after desorption 4 times.
| Number is desorbed | Operating time h | Toluene level mg/m3 |
| 0 | 2000 | 13.6 |
| 1 | 1750 | 14.1 |
| 2 | 1200 | 15.2 |
| 3 | 900 | 15.6 |
| 4 | 300 | 16.9 |
Embodiment 5
0.5mol/L nitric acid solution is prepared, passes through the fluidization wash formal layout active carbon of active carbon bed using pickling solution,
Treatment fluid liquid hourly space velocity (LHSV) 30h-1, 40 DEG C of temperature, time 1h.After filter, be washed with deionized to pH be 6, in 60 DEG C of items
Dry 12h, obtains nitric acid and washes rear active carbon under part.0.1mol/L liquor potassic permanganate is prepared, nitric acid is washed into rear active carbon and is placed in material
In tank, agitator treating mode is loaded in liquor potassic permanganate, and load liquid and active carbon volume ratio are 3:1, mixing speed 200r/
Min, 25 DEG C of temperature, time 4h.After filter, in 300 DEG C of roasting 6h, aromatic hydrocarbon substance adsorbent is made, sample characterization is such as
Shown in following table:
10wt/a producing cyclohexane by benzene hydrogenation process units, tail gas enter 800mg/m containing benzene before absorbing unit3Exhaust flow 600m3/
H, absorbing unit loadings 5t, empties after adsorbing, wherein benzene=1.7mg/m3.After operating time 1800h, benzene=4.3mg/m3,
Close to limited value of discharge standard, 2h are desorbed using 150 DEG C of steam in adsorbent after use desorption, after nitrogen purge 2h.It repeats
Desorption number see the table below with operating time, replace adsorbent after desorption 4 times.
| Number is desorbed | Operating time h | Benzene content mg/m3 |
| 0 | 1800 | 4.3 |
| 1 | 1500 | 5.1 |
| 2 | 1100 | 5.6 |
| 3 | 600 | 6.5 |
| 4 | 200 | 6.8 |
Claims (10)
1. it is a kind of for adsorbing the adsorbent of aromatic hydrocarbon substance, it is characterized in that it is carrier, specific surface area that adsorbent, which selects active carbon,
≥680m2•g-1, granularity is 5-8 mesh, Kong Rongwei 0.27-0.35cm3•g-1, aperture is micropore 1.2-1.7nm, and surface manganese contains
Amount >=2.0%, section manganese content >=1.0%.
2. according to claim 1 for adsorbing the preparation method of the adsorbent of aromatic hydrocarbon substance, it is characterized in that adsorbent selects
It is carrier with active carbon, first prepares oxyacid soln, active carbon pickling is filtered, washed to pH value 6-7, dry at 60-120 DEG C
Dry 6-12h；Salting liquid containing manganese Metal is prepared, active carbon passes through the load of salting liquid containing manganese Metal, filtering, in 300- by treated
2-6h is roasted under the conditions of 600 DEG C, and adsorbent is made after roasting.
3. according to claim 2 for adsorbing the preparation method of the adsorbent of aromatic hydrocarbon substance, it is characterized in that oxyacid is molten
Liquid be concentration be 0.5-5mol/L nitric acid, phosphoric acid, formic acid, one or more of acetic acid.
4. according to claim 2 for adsorbing the preparation method of the adsorbent of aromatic hydrocarbon substance, it is characterized in that active carbon
Pickling mode are as follows: fluidization wash of the pickling solution by active carbon bed, treatment fluid liquid hourly space velocity (LHSV) 30-60h-1, temperature 20-40
DEG C, time 0.5-1h.
5. according to claim 2 for adsorbing the preparation method of the adsorbent of aromatic hydrocarbon substance, it is characterized in that active carbon
Pickling mode are as follows: active carbon is placed in batch can, and batch can is placed in acid solution and stirs, and pickling solution and active carbon volume ratio are 3:1-6:1,
Mixing speed 200-400r/min.
6. according to claim 2 for adsorbing the preparation method of the adsorbent of aromatic hydrocarbon substance, it is characterized in that active carbon
Pickling mode are as follows: stewing process, pickling solution liquid and active carbon volume ratio are 1.5:1-2:1,30-60 DEG C of temperature, time 8-12h.
7. according to claim 2 for adsorbing the preparation method of the adsorbent of aromatic hydrocarbon substance, it is characterized in that described contain manganese
The manganese content of metal salt solution is 0.1-0.4mol/L；The salting liquid containing manganese Metal is potassium permanganate, sodium permanganate, nitric acid
One or more of manganese, manganese acetate.
8. according to claim 2 for adsorbing the preparation method of the adsorbent of aromatic hydrocarbon substance, it is characterized in that described will place
Active carbon after reason passes through the mode of loading of salting liquid containing manganese Metal are as follows: treatment fluid is born by the fluidization wash of active carbon bed
Carrier fluid liquid hourly space velocity (LHSV) 10-30h-1, 20-40 DEG C of temperature, time 1-2h.
9. according to claim 2 for adsorbing the preparation method of the adsorbent of aromatic hydrocarbon substance, it is described will that treated be living
Property charcoal pass through the mode of loading of salting liquid containing manganese Metal are as follows: active carbon is placed in batch can, the agitator treating in treatment fluid, load liquid
Volume and active carbon volume ratio are 3:1-6:1, mixing speed 200-300r/min, 20-40 DEG C of temperature, time 4-8h.
10. according to claim 2 for adsorbing the preparation method of the adsorbent of aromatic hydrocarbon substance, it is described will that treated be living
Property charcoal pass through the mode of loading of salting liquid containing manganese Metal are as follows: stand, treatment fluid volume and active carbon volume ratio are 2:1-4:1, temperature
20-40 DEG C, time 10-16h.
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| CN110898804A (en) * | 2019-11-25 | 2020-03-24 | 湖南第一师范学院 | Biochar composite material and preparation method and application thereof |
| CN114931927A (en) * | 2022-05-04 | 2022-08-23 | 中海油天津化工研究设计院有限公司 | Adsorbent for adsorbing and separating aromatic hydrocarbons in gasoline and diesel oil and preparation method thereof |
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