CN108554368A - A kind of preparation method and application of the adsorbent of removing low concentration hydrogen sulphide - Google Patents
A kind of preparation method and application of the adsorbent of removing low concentration hydrogen sulphide Download PDFInfo
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- CN108554368A CN108554368A CN201810380185.1A CN201810380185A CN108554368A CN 108554368 A CN108554368 A CN 108554368A CN 201810380185 A CN201810380185 A CN 201810380185A CN 108554368 A CN108554368 A CN 108554368A
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
- B01J20/3204—Inorganic carriers, supports or substrates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/304—Hydrogen sulfide
Abstract
The invention discloses a kind of preparation method and applications of the adsorbent of removing low concentration hydrogen sulphide, using boehmite as carrier, sesbania powder is added to be blended as binder, then by impregnating soluble alkali metal salts solution, catalyst precarsor is obtained, then the efficient bar shaped load type adsorbing agent of removing hydrogen sulfide is made after extruded moulding, drying, roasting.The adsorbent of the present invention belongs to dry-desulphurizer, overcomes in wet method and is not suitable with the removing of low concentration hydrogen sulphide with liquid-absorbant to remove sulfide equipment treating capacity big, investment and larger, cumbersome, efficiency the is low problem of operating cost, especially wet method；And the adsorbent has the characteristics that adsorption of Low Concentration hydrogen sulfide is efficient, intensity is high, at low cost, equipment investment is low, non-secondary pollution, is easy to industrialized production.
Description
Technical field
The invention belongs to adsorbent preparing technical fields, and in particular to a kind of system of the adsorbent of removing low concentration hydrogen sulphide
Preparation Method and application.
Background technology
Hydrogen sulfide is a kind of irritative gas with strong rotten egg smell, and odor pollution have been considered as it is only secondary
In one of the six big public hazards of noise；Or a kind of strong neurotoxic substance, can directly be detrimental to health.It is to cause air dirty
Dye, greenhouse effects and one of the main matter for destroying ozone layer.The hazard profile of hydrogen sulfide is embodied in：Toxic, combustion
It is quick-fried property, corrosivity, diffusivity, agility, calamitous.China is dense to hydrogen sulfide in ambient air, workshop air and industrial waste gas
There are strict requirements for degree：The maximum concentration of hydrogen sulfide must not exceed 0.01 mg/m in the ambient air of residential block3；Shopwork
Point Air Hydrogen Sulfide maximum concentration must not exceed 10 mg/m3；Concentration of hydrogen sulfide must not exceed 20 mg/m in town gas3；Oil
Concentration of hydrogen sulfide requires purification to 10~20 mg/m in product refinery off gas3.Hydrogen sulfide gas, which is administered, especially vulcanizes low concentration
The improvement of hydrogen Treatment process and the exploitation of new technology, become current urgent problem to be solved.In recent years, domestic and foreign scholars couple
The removing research of low concentration hydrogen sulphide expands a large amount of research work.
So far, removing low concentration hydrogen sulphide technique includes wet method and dry method two major classes, and wet processing includes absorption process
And wet oxidation process.Wet processing generally uses absorbing liquid to remove hydrogen sulfide, disposably can convert hydrogen sulfide to elemental sulfur,
Equipment treating capacity is big, investment and operating cost are small, can operate continuously, but efficiency is low, is difficult to reach high requirement, while generating corruption
The series of problems such as erosion, fouling.During the sulfur removal technology of dry desulfurization, gas-solid occurs and is in contact reaction, i.e., using powdery or
Hydrogen sulfide gas is adsorbed or reacted by the desulfurizing agent of grain is fixed as solid sulphur, and reaction is carried out in the state of being completely dried
, because without there is the series of problems such as corrosion and scaling.Dry desulfurization is also known as absorption method.Common adsorbent can be divided into activity
Charcoal, iron oxide, molecular sieve etc..
Activated carbon pore structure is flourishing, has huge specific surface area, in gas, solution inorganic or organic substance and
Colloidal solid etc. has very strong adsorption capacity.The secondary desulfuration that active carbon desulfurization is primarily adapted for use in room temperature range feed gas is gentle
The removing of body sulfide.But because of its catalytic oxidation desulfurization mechanism, it need to be operated in the case where there is oxygen atmosphere, there is the later stage in use
The problem of desulfurization.Activated carbon adsorption treatment process is easy hardened, large specific surface area the problem is that activated carbon is met after water makes moist
It is big to reduce, to influence treatment effect.After activated carbon surface adsorbs excessive pollutant, efficiency can also reduce, to one
It must just replace, regenerate when determining degree.
Iron oxide is reacted with hydrogen sulfide generates iron sulfide and water, can be divided into middle low-temp desulfurization and high temperature desulfurizing.Middle low temperature is de-
Sulphur technique has industrialized, and high temperature desulfurizing is still at the experimental stage.Single metal oxides method is that one is used in sweetening process
The single metal oxide of kind removes the sulfur-containing impurities such as hydrogen sulfide gas as desulfurizing agent main body.Current maximum difficult point is
Pulverizing problem in ferric oxide desulfurizer recycling.
Application of the molecular sieve in gas separation and purification process is a kind of emerging technology in recent years, its selectivity is good,
It is active high, catalyst or catalyst carrier are often used as in adsorption process, adsorbent of molecular sieve is widely used in removing gas
In hydrogen sulfide.Regenerating molecular sieve can be used 200~300 DEG C, since molecular sieve is also steady under 550 DEG C or higher temperature
Fixed, and regenerate completely, therefore the service life is very long, but have the shortcomings that regeneration energy consumption is big.
Boehmite is a kind of white powder, has that specific surface area is high, colloidal sol is good, caking property is strong, large pore volume etc. is excellent
Point is widely used in the fields such as catalyst, catalyst carrier, adsorbent.
Currently, dry desulfurizing process there is a problem in production cost, control side reaction and stability etc..It opens
The adsorbent that it is cheap to send out a kind of, efficient, composition is simple, stability is good is for removing the protrusion that low concentration hydrogen sulphide is still development
Hot spot.
Invention content
Present invention aim to address be used to remove adsorption of Low Concentration sulphur existing for the adsorbent of hydrogen sulfide in the prior art
Change low, the unstable problem of hydrogen efficiency, and then provides a kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide and answer
With.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide, using boehmite after pretreatment as carrier, so
Soluble alkali metal salts solution is impregnated afterwards, specifically includes following steps：
(1) pretreatment of boehmite：Industrial boehmite is ground to powder, is dried in an oven, it is dry
Temperature is 50~100 DEG C, 5~24 h of drying time, removes surface Free water, the boehmite after handling is as carrier；
(2) binder is added：Sesbania powder is added by being mixed together as binder in pretreated boehmite powder
Uniformly, sesbania powder and the mass ratio by pretreated boehmite powder are 1:10~1:100, obtain boehmite and
Sesbania powder mixed-powder；
(3) soluble alkali metal salts solution is added in deionized water, soluble alkali metal salts solution is obtained after being sufficiently stirred；
The mass ratio of boehmite carrier after the soluble alkali metal salts and pretreatment is 1:1~1:10；
(4) boehmite obtained in step (2) and sesbania is added in the soluble alkali metal salts solution that step (3) obtains
In powder mixed-powder, homogeneous impregnation obtains catalyst precarsor；
(5) catalyst precarsor is placed in banded extruder and is molded, obtain bar shaped sample；
(6) by sample after molding, the adsorbent of removing hydrogen sulfide is obtained after drying, calcination process.
Soluble alkali metal salts solution described in step (3) is that sodium hydroxide, sodium carbonate, the alkali metal salt of potassium carbonate are molten
The mixture of one or more of liquid；It is furthermore preferred that used soluble alkali metal salts solution is sodium carbonate liquor.
Soluble metal salt solution described in step (4), which is added in boehmite and sesbania powder mixed-powder, to be impregnated
Method to catalyst precarsor is preferably incipient impregnation.
In step (6), the technological parameter of the drying process is：Drying temperature is 80~200 DEG C, drying time 10
~30 h；The technological parameter of calcination process is：Calcination temperature is 400~700 DEG C, and roasting time is 2~8 h.
By adsorbent obtained above for removing low concentration hydrogen sulphide reaction, the condition of absorption：Gas hydrogen sulfide concentration
For：10~500 ppm；Reaction temperature is：10~60 ℃；Pressure is 0 ~ 2 Mpa；Reaction flow velocity is 10~150 ml/min.
The beneficial effects of the present invention are：Adsorbent produced by the present invention belongs to dry-desulphurizer, overcome in wet method with
Liquid-absorbant removes sulfide equipment treating capacity big, investment and larger, cumbersome, efficiency the is low problem of operating cost,
Especially wet method is not suitable with the removing of low concentration hydrogen sulphide；And the adsorbent has adsorption of Low Concentration hydrogen sulfide efficient, strong
Degree is high, feature at low cost, and equipment investment is low, non-secondary pollution, is easy to industrialized production.
Description of the drawings
Fig. 1 is the XRD spectra of the adsorbent of different sodium carbonate load percentages produced by the present invention；
Fig. 2 is that the adsorbent of different sodium carbonate load percentages produced by the present invention absorbs H2The breakthrough curve of S gases compares figure.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
A kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide described in the present embodiment, includes the following steps：
50.00 g boehmites accurately are weighed, powder is ground to and is put into 200 ml porcelain member wares, be then placed on 60 DEG C
Dry 12 h, remove surface Free water, the boehmite after handling is as carrier in baking oven；Accurately weigh 1.75 g sesbanias
Powder is added by being mixed together as binder in pretreated boehmite powder, and mechanical agitation is uniform, obtains intending thin water
Aluminium stone and sesbania powder mixed-powder；50 g sodium carbonate are weighed, is added in 50 g deionized waters, sodium carbonate salt is obtained after being sufficiently stirred
Solution；Sodium carbonate salt solution is slowly added into boehmite and sesbania powder mixed-powder, homogeneous impregnation obtains catalyst
Precursor；Catalyst precarsor is placed on a diameter of 1.5 mm of shaped granule in banded extruder；By sample after molding, through 100 DEG C of dryings
12 h；500 DEG C of 4 h of roasting are to get to Na2CO3:AlOOH=1:1 adsorbent, working sulfur capacity are listed in Table 1 below.
Embodiment 2
A kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide described in the present embodiment, includes the following steps：
50.00 g boehmites accurately are weighed, powder is ground to and is put into 200 ml porcelain member wares, be then placed on 60 DEG C
Dry 12 h, remove surface Free water, the boehmite after handling is as carrier in baking oven；Accurately weigh 1.75 g sesbanias
Powder is added by being mixed together as binder in pretreated boehmite powder, and mechanical agitation is uniform, obtains intending thin water
Aluminium stone and sesbania powder mixed-powder；25 g sodium carbonate are weighed, is added in 50 g deionized waters, sodium carbonate salt is obtained after being sufficiently stirred
Solution；Sodium carbonate salt solution is slowly added into boehmite and sesbania powder mixed-powder, homogeneous impregnation obtains catalyst
Precursor；Catalyst precarsor is placed on a diameter of 1.5 mm of shaped granule in banded extruder；By sample after molding, through 100 DEG C of dryings
12 h；500 DEG C of 4 h of roasting are to get to Na2CO3:AlOOH=1:2 adsorbent, working sulfur capacity are listed in Table 1 below.
Embodiment 3
A kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide described in the present embodiment, includes the following steps：
50.00 g boehmites accurately are weighed, powder is ground to and is put into 200 ml porcelain member wares, be then placed on 100 DEG C
Dry 12 h, remove surface Free water, the boehmite after handling is as carrier in baking oven；Accurately weigh 1.75 g sesbanias
Powder is added by being mixed together as binder in pretreated boehmite powder, and mechanical agitation is uniform, obtains intending thin water
Aluminium stone and sesbania powder mixed-powder；12.5 g sodium carbonate are weighed, is added in 50 g deionized waters, sodium carbonate is obtained after being sufficiently stirred
Salting liquid；Sodium carbonate salt solution is slowly added into boehmite and sesbania powder mixed-powder, homogeneous impregnation is catalyzed
Agent precursor；Catalyst precarsor is placed on a diameter of 1.5 mm of shaped granule in banded extruder；It is dry through 100 DEG C by sample after molding
Dry 12 h；450 DEG C of 4 h of roasting are to get to Na2CO3:AlOOH=1:4 adsorbent, working sulfur capacity are listed in Table 1 below.
Embodiment 4
A kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide described in the present embodiment, includes the following steps：
50.00 g boehmites accurately are weighed, powder is ground to and is put into 200 ml porcelain member wares, be then placed on 80 DEG C
Dry 12 h, remove surface Free water, the boehmite after handling is as carrier in baking oven；Accurately weigh 1.75 g sesbanias
Powder is added by being mixed together as binder in pretreated boehmite powder, and mechanical agitation is uniform, obtains intending thin water
Aluminium stone and sesbania powder mixed-powder；8.3 g sodium carbonate are weighed, is added in 50 g deionized waters, sodium carbonate is obtained after being sufficiently stirred
Salting liquid；Sodium carbonate salt solution is slowly added into boehmite and sesbania powder mixed-powder, homogeneous impregnation is catalyzed
Agent precursor；Catalyst precarsor is placed on a diameter of 1.5 mm of shaped granule in banded extruder；It is dry through 100 DEG C by sample after molding
Dry 12 h；550 DEG C of 4 h of roasting are to get to Na2CO3:AlOOH=1:6 adsorbent, working sulfur capacity are listed in Table 1 below.
1 working sulfur capacity of table compares
H is carried out to the sorbent material prepared by above-described embodiment 1-42The breakthrough experiment of S gases measures and to embodiment 1-4 institute
The sorbent material of preparation does XRD characterization.Fig. 1 is the XRD spectrums of the adsorbent of different sodium carbonate load percentages produced by the present invention
Figure.It can be seen that the increase with load percentage, the peak intensity of aluminium hydroxide and crystal carbonate is remarkably reinforced, 1:Reach when 2
Maximum, corresponding working sulfur capacity are also maximum.
Fig. 2 is that the adsorbent of different sodium carbonate load percentages produced by the present invention absorbs H2The breakthrough curve of S gases.Test
Condition is：2.23 g adsorbents are fitted into quartz ampoule fixed bed reactors, hydrogen sulfide gas entrance concentration is：100 ppm；Instead
The temperature is answered to be：20 ℃；Pressure is 0.01 Mpa.Sampling in every 30 minutes is primary, it is specified that it is to wear that concentration of hydrogen sulfide, which reaches 0.1 ppm,
Saturating Sulfur capacity；It is saturation Sulfur capacity that concentration of hydrogen sulfide, which reaches 100 ppm,.
Sulfur capacity calculation formula is；
Wherein, Y is working sulfur capacity, mg/mL；V is gas flow, mL/min；T is time of break-through, min；C0For entrance H2S is dense
Degree, %；C is outlet H2S concentration, %；G is fresh desulfurizing agent volume, ml, M=34 g/mol, Vm=22.4 mL/mol.Utilize Japan
Import sulfurated hydrogen detection pipe, sensitivity are accurate to 0.1 ppm.The adsorbent that as can be seen from Figure 2 prepared by the present invention has very
High absorption property, and, time of break-through longest best with the adsorbent absorption property prepared by embodiment 2.
In conclusion the adsorbent of the removing low concentration hydrogen sulphide prepared using the present invention, time of break-through is long, adsorption effect
It is good, hence it is evident that higher than having industrialized same type adsorbent.
The above embodiments are merely examples for clarifying the description, and does not limit the embodiments.For institute
For the those of ordinary skill in category field, other various forms of variations or change can also be made on the basis of the above description
It is dynamic.Here all embodiments can not be also exhaustive.Rather than changes and variations that derived from are still located
Among the protection domain of the invention.
Claims (8)
1. a kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide, it is characterised in that：It is preprocessed with boehmite
It is used as carrier afterwards, then impregnates soluble alkali metal salts solution, specifically includes following steps：
(1) pretreatment of boehmite：Industrial boehmite is ground to powder, is dried in an oven, is removed
Surface Free water, the boehmite after handling is as carrier；
(2) binder is added：Sesbania powder is added by being mixed together as binder in pretreated boehmite powder
Uniformly, boehmite and sesbania powder mixed-powder are obtained；
(3) soluble alkali metal salts are added in deionized water, soluble alkali metal salts solution is obtained after being sufficiently stirred；
(4) boehmite obtained in step (2) and sesbania powder is added in the soluble alkali metal salts solution that step (3) obtains
In mixed-powder, homogeneous impregnation obtains catalyst precarsor；
(5) catalyst precarsor is placed in banded extruder and is molded, obtain sample after molding；
(6) by sample after molding, the adsorbent of removing hydrogen sulfide is obtained after dry and calcination process.
2. a kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide according to claim 1, it is characterised in that：
The technological parameter of the preprocessing process of boehmite is in the step (1)：Drying temperature is 50~100 DEG C, drying time
5~24 h.
3. a kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide according to claim 1, it is characterised in that：
In the step (2), sesbania powder and the mass ratio by pretreated boehmite powder are 1:10~1:100.
4. a kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide according to claim 1, it is characterised in that：
The mass ratio of boehmite carrier after the soluble alkali metal salts and pretreatment is 1:1~1:10.
5. a kind of preparation method of the adsorbent of removing low concentration hydrogen sulphide according to claim 1, it is characterised in that：
Soluble alkali metal salts solution described in step (3) is one kind in the metal salt solution of sodium hydroxide, sodium carbonate, potassium carbonate
Or it is several.
6. the preparation method of the adsorbent of removing low concentration hydrogen sulphide according to claim 1, it is characterised in that：Step
(4) dipping method described in is incipient impregnation.
7. the preparation method of the adsorbent of removing low concentration hydrogen sulphide according to claim 1, it is characterised in that：Step
(6) in, the technological parameter of the drying process is：Drying temperature is 80~200 DEG C, and drying time is 10~30 h；The roasting
Burning the technological parameter handled is：Calcination temperature is 400~700 DEG C, and roasting time is 2~8 h.
8. a kind of application of the adsorbent as made from preparation method according to any one of claims 1 to 7, it is characterised in that：
The adsorbent is reacted for carrying out removing low concentration hydrogen sulphide, and process conditions are：Gas hydrogen sulfide concentration is：10~500
ppm；Reaction temperature is：10~60 ℃；Pressure is 0 ~ 2 Mpa；Reaction flow velocity is 10~150 ml/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109482134A (en) * | 2018-12-29 | 2019-03-19 | 山东华泰纸业股份有限公司 | A kind of preparation method of micro/nano level desulfuration adsorbent |
| CN110882675A (en) * | 2019-12-17 | 2020-03-17 | 西北化工研究院有限公司 | Preparation method of renewable hydrogen sulfide gas adsorbent |
| CN115400720A (en) * | 2022-08-26 | 2022-11-29 | 华南师范大学 | Adsorbent for removing sulfur-containing malodorous gas in non-ferrous metal mining area and preparation method and application thereof |
| US11745162B2 (en) | 2020-11-29 | 2023-09-05 | Shanghai Lvqiang New Materials Co., Ltd | Regenerable hydrogen sulfide adsorbent and preparation method thereof and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109482134A (en) * | 2018-12-29 | 2019-03-19 | 山东华泰纸业股份有限公司 | A kind of preparation method of micro/nano level desulfuration adsorbent |
| CN110882675A (en) * | 2019-12-17 | 2020-03-17 | 西北化工研究院有限公司 | Preparation method of renewable hydrogen sulfide gas adsorbent |
| CN110882675B (en) * | 2019-12-17 | 2022-11-18 | 西北化工研究院有限公司 | Preparation method of renewable hydrogen sulfide gas adsorbent |
| US11745162B2 (en) | 2020-11-29 | 2023-09-05 | Shanghai Lvqiang New Materials Co., Ltd | Regenerable hydrogen sulfide adsorbent and preparation method thereof and application thereof |
| CN115400720A (en) * | 2022-08-26 | 2022-11-29 | 华南师范大学 | Adsorbent for removing sulfur-containing malodorous gas in non-ferrous metal mining area and preparation method and application thereof |
| CN115400720B (en) * | 2022-08-26 | 2023-10-27 | 华南师范大学 | Adsorbent for removing sulfur-containing malodorous gas in nonferrous metal mining area and preparation method and application thereof |
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Application publication date: 20180921 |