CN106914213A - A kind of natural gas mercury-removing adsorbent and preparation method thereof - Google Patents
A kind of natural gas mercury-removing adsorbent and preparation method thereof Download PDFInfo
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- CN106914213A CN106914213A CN201510999784.8A CN201510999784A CN106914213A CN 106914213 A CN106914213 A CN 106914213A CN 201510999784 A CN201510999784 A CN 201510999784A CN 106914213 A CN106914213 A CN 106914213A
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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
- 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
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
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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
- B01J20/0274—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 characterised by the type of anion
- B01J20/0285—Sulfides of compounds other than those provided for in B01J20/045
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
- C10L2290/542—Adsorption of impurities during preparation or upgrading of a fuel
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Abstract
The present invention relates to a kind of natural gas mercury-removing adsorbent and preparation method thereof, belong to demercuration adsorbent field.Natural gas mercury-removing adsorbent includes active component and carrier, and the weight of active component accounts for the 8~27% of demercuration adsorbent gross weight, and active component is the sulfide of copper, and carrier is active alundum (Al2O3).(1) basic copper carbonate is dissolved in the mixed solution of ammoniacal liquor or unsaturated carbonate hydrogen ammonium salt solution or ammoniacal liquor with unsaturated carbonate hydrogen ammonium, as modified solution；(2) active alumina carrier is immersed in above-mentioned modified solution, the active alumina carrier of loaded modified solution is leached, drained or dried at 80~150 DEG C；(3) above-mentioned dried carrier is calcined at 180~240 DEG C, obtains demercuration adsorbent precursor；(4) above-mentioned demercuration adsorbent precursor is vulcanized, obtains demercuration adsorbent.Obtained natural gas mercury-removing adsorbent of the invention is cheap, to environment non-secondary pollution, has removal efficiency higher to the mercury in natural gas.
Description
Technical field
The present invention relates to a kind of natural gas mercury-removing adsorbent and preparation method thereof, belong to demercuration adsorbent field.
Background technology
All contain mercury in many natural gas gas reservoirs in the world, mercury is the trace non-hydrocarbons group of generally existing in natural gas
Point, its changes of contents scope is very big, it is considered that in 1~200 μ g/m3Between.Mercury in natural gas it is main with
The form of elemental is present, and exists in forms such as the mercurides of organic mercury, inorganic mercury salt and suspension on a small quantity.Mercury and
Its compound is extremely toxic substance, and operation and maintainer may be good for during mercurous natural gas processing
Health constitutes harm, and mercury can also occur amalgam reaction with the metal for contacting, and amalgam has stronger brittle behavior,
Long term accumulation can cause the destruction of process equipment, and the destruction especially for aluminium heater is particularly acute.And, day
Mercury in right gas can be discharged into surrounding environment by three kinds of channels such as waste water, solid waste and gas escape
Cause serious mercury pollution problem.Also, associated mechanisms research shows, the content of Hg in natural gas is less than 30
μg/m3When, substantially harm will not be caused to equipment, personal safety, environment.China's oil industry Recommendations
Mercury content is less than 28 μ g/m in pipeline gas3.Therefore, consider that exploitation has hair from factors such as environmental protection, safety
The natural gas mercury-removing adsorbent of exhibition prospect, is necessary, especially effectively to remove the mercury in natural gas
It is the mercury (Hg of elemental form0) it is one of environmental pollution improvement's urgent problem.
China starts late for the research and development of demercuration adsorbent, and current state's interior energy produces the enterprise of demercuration adsorbent
It is less, and the demercuration adsorbent generally existing service life of domestic production is short, mercury holds and demercuration efficiency is all smaller
The problems such as.Also, the country is relatively low for the Innovation Input of mercury removal agent, the reason such as technology and adequate and systematic service backwardness
It is difficult to be competed with offshore company, the domestic demercuration adsorbent major part for using is caused to also need to rely on import.
The content of the invention
It is high it is an object of the invention to provide a kind of demercuration efficiency and do not produce the natural of secondary pollution again based on this
Qi exhaustion mercury absorbent and preparation method thereof.
To achieve the above object, the technical scheme is that：
A kind of natural gas mercury-removing adsorbent, the adsorbent includes active component and carrier, the weight of the active component
Amount accounts for the 8~27% of natural gas mercury-removing total sorbent weight, and the active component is the sulfide of copper, the load
Body is active alundum (Al2O3).
The preparation method of described natural gas mercury-removing adsorbent, comprises the following steps：
(1) basic copper carbonate is dissolved completely in ammoniacal liquor or unsaturated carbonate hydrogen ammonium salt solution or ammoniacal liquor and unsaturated carbonate hydrogen
In the mixed solution of ammonium, as modified solution；
(2) active alumina carrier is immersed in above-mentioned modified solution, by loaded modified dose of active three oxygen
Change two alumina supporters to leach, dry；
(3) by the above-mentioned active alumina carrier for drying back loading modifying agent, roasted at 180~240 DEG C
Burn, obtain demercuration adsorbent precursor；
(4) above-mentioned demercuration adsorbent precursor is vulcanized, obtains natural gas mercury-removing adsorbent.
The preparation method of described natural gas mercury-removing adsorbent, in step (1), copper ion is dense in modified solution
It is 1~4.5mol/L to spend.
The preparation method of described natural gas mercury-removing adsorbent, in step (2), active alumina carrier
Particle diameter is 1.5~4.5mm, effective pore volume is 0.75~0.95cm3/ g, specific surface area are 150~300m2/g。
The preparation method of described natural gas mercury-removing adsorbent, in step (2), when loaded modified dose of activity three
After Al 2 O carrier is drained, then 1~4h of forced air drying at 80~150 DEG C.
The preparation method of described natural gas mercury-removing adsorbent, in step (3), roasting is carried out under the conditions of air blast.
The preparation method of described natural gas mercury-removing adsorbent, in step (4), the vulcanizing agent that vulcanization is used is sulphur
Change hydrogen, any one in the ammonium sulfide solution that sulfur content is 5~15wt%.
The preparation method of described natural gas mercury-removing adsorbent, in step (4), through the demercuration adsorbent after vulcanization
At 80~150 DEG C, 4~16h is dried under the conditions of air blast.
The preparation method of described natural gas mercury-removing adsorbent, in step (4), by quality ratio, natural qi exhaustion
The sulfide of copper and active alumina carrier mass ratio are (8~27) in mercury absorbent：(73~92).
The present invention has advantages below and beneficial effect：
1st, the present invention is using unique modified solution, the demercuration adsorbent for preparing under given conditions, tool
There are larger pore volume, specific surface area and active component content, and then the removal efficiency of demercuration adsorbent can be improved.
2nd, in the preparation method of natural gas mercury-removing adsorbent of the present invention, further control is right under the conditions of air blast
The active alumina carrier of loaded modified solution is dried, so as to remain the pore volume of carrier, further
Ensure the vulcanization rate of copper compound in mercury removal agent precursor, so as to improve the demercuration efficiency of demercuration adsorbent.
3rd, the obtained natural gas mercury-removing adsorbent of the present invention is cheap, to environment non-secondary pollution, to natural gas
In mercury have removal efficiency higher.
Specific embodiment
Below, by embodiment, the present invention is described in more detail.
Embodiment 1
The present embodiment uses and the sulfide of active ingredient copper is carried on active alumina carrier, with
To the natural gas mercury-removing adsorbent with mercury removal effect higher, comprise the following steps：
(1) basic copper carbonate is dissolved completely in ammoniacal liquor, as modified solution, copper ion in modified solution
Concentration is 2mol/L；
(2) active alumina carrier is immersed in above-mentioned modified solution, by loaded modified dose of active three oxygen
Change two alumina supporters to leach, after loaded modified dose of active alumina carrier is drained, then the drum at 100 DEG C
Air-dry dry 2h；
The particle diameter of active alumina carrier is 1.5~4.5mm, effective pore volume is 0.75~0.95cm3/ g, ratio
Surface area is 150~300m2/g。
(3) above-mentioned dried carrier is calcined at 200 DEG C, roasting is carried out under the conditions of air blast, is taken off
Mercury absorbent precursor；
(4) above-mentioned demercuration adsorbent precursor is vulcanized, the vulcanizing agent of vulcanization is hydrogen sulfide, obtains natural gas mercury-removing
Adsorbent.By quality ratio, the sulfide of copper is carried with active alundum (Al2O3) in the natural gas mercury-removing adsorbent
Body mass ratio is 25：75.
Natural gas mercury-removing adsorbent is cheap obtained in the present embodiment, to environment non-secondary pollution, to natural gas
In mercury have removal efficiency higher, demercuration efficiency be more than 95%.
Embodiment 2
The present embodiment uses and the sulfide of active ingredient copper is carried on active alumina carrier, with
To the natural gas mercury-removing adsorbent with mercury removal effect higher, comprise the following steps：
(1) basic copper carbonate is dissolved completely in unsaturated carbonate hydrogen aqueous ammonium, as modified solution, is modified
The concentration of copper ion is 3mol/L in solution；
(2) active alumina carrier is immersed in above-mentioned modified solution, by loaded modified dose of active three oxygen
Change two alumina supporters to leach, after loaded modified dose of active alumina carrier is drained, then the air blast at 90 DEG C
Dry 3h；
The particle diameter of active alumina carrier is 1.5~4.5mm, effective pore volume is 0.75~0.95cm3/ g, ratio
Surface area is 150~300m2/g。
(3) above-mentioned dried carrier is calcined at 180 DEG C, roasting is carried out under the conditions of air blast, is taken off
Mercury absorbent precursor；
(4) above-mentioned demercuration adsorbent precursor is vulcanized, the vulcanizing agent of vulcanization is hydrogen sulfide, sulfur content be 5~
Any one in the ammonium sulfide solution of 15wt%, obtains natural gas mercury-removing adsorbent.By quality ratio, it is described
The sulfide of copper and active alumina carrier mass ratio are 20 in natural gas mercury-removing adsorbent：80.
Natural gas mercury-removing adsorbent is cheap obtained in the present embodiment, to environment non-secondary pollution, to natural gas
In mercury have removal efficiency higher, demercuration efficiency be 96% or so.
Embodiment 3
The present embodiment uses and the sulfide of active ingredient copper is carried on active alumina carrier, with
To the natural gas mercury-removing adsorbent with mercury removal effect higher, comprise the following steps：
(1) basic copper carbonate is dissolved completely in mixed solution of the ammoniacal liquor with unsaturated carbonate hydrogen aqueous ammonium, ammonia
Water is 1 with the volume ratio of unsaturated carbonate hydrogen aqueous ammonium：1, as modified solution, copper ion in modified solution
Concentration is 4mol/L；
(2) active alumina carrier is immersed in above-mentioned modified solution, by loaded modified dose of active three oxygen
Change two alumina supporters to leach, after loaded modified dose of active alumina carrier is drained, then the drum at 120 DEG C
Air-dry dry 2h；
The particle diameter of active alumina carrier is 1.5~4.5mm, effective pore volume is 0.75~0.95cm3/ g, ratio
Surface area is 150~300m2/g。
(3) above-mentioned dried carrier is calcined at 220 DEG C, roasting is carried out under the conditions of air blast, is taken off
Mercury absorbent precursor；
(4) above-mentioned demercuration adsorbent precursor is vulcanized, the vulcanizing agent of vulcanization is hydrogen sulfide, sulfur content be 5~
Any one in the ammonium sulfide solution of 15wt%, obtains natural gas mercury-removing adsorbent.By quality ratio, it is described
The sulfide of copper and active alumina carrier mass ratio are 10 in natural gas mercury-removing adsorbent：90.
Natural gas mercury-removing adsorbent is cheap obtained in the present embodiment, to environment non-secondary pollution, to natural gas
In mercury have removal efficiency higher, demercuration efficiency be more than 95%.
Claims (9)
1. a kind of natural gas mercury-removing adsorbent, it is characterised in that the adsorbent includes active component and carrier, institute
The weight for stating active component accounts for the 8~27% of natural gas mercury-removing total sorbent weight, and the active component is copper
Sulfide, the carrier is active alundum (Al2O3).
2. the preparation method of the natural gas mercury-removing adsorbent described in a kind of claim 1, it is characterised in that including
Following steps：
(1) basic copper carbonate is dissolved completely in ammoniacal liquor or unsaturated carbonate hydrogen ammonium salt solution or ammoniacal liquor and unsaturated carbonate hydrogen
In the mixed solution of ammonium, as modified solution；
(2) active alumina carrier is immersed in above-mentioned modified solution, by loaded modified dose of active three oxygen
Change two alumina supporters to leach, dry；
(3) by the above-mentioned active alumina carrier for drying back loading modifying agent, roasted at 180~240 DEG C
Burn, obtain demercuration adsorbent precursor；
(4) above-mentioned demercuration adsorbent precursor is vulcanized, obtains natural gas mercury-removing adsorbent.
3. the preparation method of natural gas mercury-removing adsorbent according to claim 2, it is characterised in that step
(1) in, the concentration of copper ion is 1~4.5mol/L in modified solution.
4. the preparation method of natural gas mercury-removing adsorbent according to claim 2, it is characterised in that step
(2) in, the particle diameter of active alumina carrier is 1.5~4.5mm, effective pore volume is 0.75~0.95cm3/g、
Specific surface area is 150~300m2/g。
5. the preparation method of natural gas mercury-removing adsorbent according to claim 2, it is characterised in that step
(2) in, after loaded modified dose of active alumina carrier is drained, then air blast is done at 80~150 DEG C
Dry 1~4h.
6. the preparation method of natural gas mercury-removing adsorbent according to claim 2, it is characterised in that step
(3) in, roasting is carried out under the conditions of air blast.
7. the preparation method of natural gas mercury-removing adsorbent according to claim 2, it is characterised in that step
(4) in, appointing in vulcanizing the vulcanizing agent for using for the ammonium sulfide solution that hydrogen sulfide, sulfur content are 5~15wt%
Meaning is a kind of.
8. the preparation method of natural gas mercury-removing adsorbent according to claim 2, it is characterised in that step
(4) in, through the demercuration adsorbent after vulcanization at 80~150 DEG C, 4~16h is dried under the conditions of air blast.
9. the preparation method of the natural gas mercury-removing adsorbent according to Claims 2 or 3, it is characterised in that
In step (4), by quality ratio, the sulfide of copper is carried with active alundum (Al2O3) in natural gas mercury-removing adsorbent
Body mass ratio is (8~27)：(73~92).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107486133A (en) * | 2017-09-12 | 2017-12-19 | 常州大学 | A kind of natural gas mercury-removing adsorbent and preparation method |
| CN111394144A (en) * | 2020-03-13 | 2020-07-10 | 山西新华化工有限责任公司 | Mercury remover and preparation method thereof |
| US10843182B2 (en) | 2017-11-17 | 2020-11-24 | Industrial Technology Research Institute | Composite material comprising porous silicate particles and active metals |
| CN115608320A (en) * | 2022-09-19 | 2023-01-17 | 四川澳凯化工有限公司 | Preparation method of mercury removal agent with desulfurization effect |
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| CN103372418A (en) * | 2012-04-28 | 2013-10-30 | 东南大学 | Modified activated carbon demercuration adsorbent and preparation method thereof |
| CN103521166A (en) * | 2013-10-22 | 2014-01-22 | 北京三聚环保新材料股份有限公司 | Preparation method of copper-based mercury removing agent |
| CN103521165A (en) * | 2013-10-22 | 2014-01-22 | 北京三聚环保新材料股份有限公司 | Preparation method of copper-based mercury removing agent |
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| CN103372418A (en) * | 2012-04-28 | 2013-10-30 | 东南大学 | Modified activated carbon demercuration adsorbent and preparation method thereof |
| CN103331140A (en) * | 2013-06-24 | 2013-10-02 | 广东电网公司电力科学研究院 | Demercuration adsorbent and preparation method thereof |
| CN103521166A (en) * | 2013-10-22 | 2014-01-22 | 北京三聚环保新材料股份有限公司 | Preparation method of copper-based mercury removing agent |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107486133A (en) * | 2017-09-12 | 2017-12-19 | 常州大学 | A kind of natural gas mercury-removing adsorbent and preparation method |
| CN107486133B (en) * | 2017-09-12 | 2019-12-31 | 常州大学 | Natural gas demercuration adsorbent and preparation method thereof |
| US10843182B2 (en) | 2017-11-17 | 2020-11-24 | Industrial Technology Research Institute | Composite material comprising porous silicate particles and active metals |
| CN111394144A (en) * | 2020-03-13 | 2020-07-10 | 山西新华化工有限责任公司 | Mercury remover and preparation method thereof |
| CN115608320A (en) * | 2022-09-19 | 2023-01-17 | 四川澳凯化工有限公司 | Preparation method of mercury removal agent with desulfurization effect |
| CN115608320B (en) * | 2022-09-19 | 2024-05-07 | 成华区雾夜话辛工程管理部 | Preparation method of mercury removal agent with desulfurization effect |
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