CN108456574A - A kind of mercury removal agent and preparation method thereof for moisture demercuration - Google Patents
A kind of mercury removal agent and preparation method thereof for moisture demercuration Download PDFInfo
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- CN108456574A CN108456574A CN201810325907.3A CN201810325907A CN108456574A CN 108456574 A CN108456574 A CN 108456574A CN 201810325907 A CN201810325907 A CN 201810325907A CN 108456574 A CN108456574 A CN 108456574A
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- Prior art keywords
- removal agent
- mercury removal
- solution
- moisture
- demercuration
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Classifications
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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
-
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/64—Heavy metals or compounds thereof, e.g. mercury
-
- 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
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/20—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by expressing the material, e.g. through sieves and fragmenting the extruded length
-
- 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
Abstract
The present invention provides a kind of mercury removal agent for moisture demercuration, including active material, carrier granular and auxiliary element；The active material is metal sulfide, wherein mass fraction >=80% of copper sulfide；The carrier granular includes activated alumina, cocoanut active charcoal and adhesion promoter；The auxiliary element is silver sulfide；The active material and auxiliary element are supported in carrier granular；The present invention also provides a kind of preparation methods of above-mentioned mercury removal agent, include the following steps：Activated alumina, cocoanut active charcoal and adhesion promoter are mixed, carrier granular is made after extrusion forming, drying；Carrier granular is impregnated into containing Cu2+And Ag+Solution in, dipping, which is placed on to calcine at 500~800 DEG C completely, is made mercury removal agent precursor；Mercury removal agent precursor is impregnated into 2~4h in sulfide solution, vulcanization, which is placed on to calcine at 500~800 DEG C, is made mercury removal agent, and the mercury removal agent is identical in copper sulfide load capacity, has better demercuration performance.
Description
Technical field
The present invention relates to mercury removal technical field, specifically a kind of mercury removal agent and preparation method thereof for moisture demercuration.
Background technology
Mercury and mercuric compounds are present in the form of pollutant in the fossil fuels such as natural gas, such as the mercury content in natural gas
Generally 1~2000 μ g/m3.Mercury has toxicity, corrosivity and bioaccumulation, and the mercury in natural gas can corroded pipeline and equipment
(especially low temperature aluminum appliance), seriously threatens the life of animals and plants, increases the risk of plant maintenance.Pipeline gas user closes
It is same to require mercury content in commercial natural gas that be less than 0.01 μ g/m3, mercury content must be low in LNG factories clear stipulaties feed natural gas
In 0.01 μ g/m3, China provides that the maximum permissible concentration that mercury enters air by modes such as burning waste gas, leakages is 15 μ g/m3。
Therefore, it is to reduce mercury in natural gas processing plant while to meet gas product quality to equipment, pipeline and the harm of operating personnel
It is required that mercury that should as possible in treatment plant's upstream removing natural gas, to mercurous gas field, reasonable, security development has great meaning for this
Justice.
Currently, the load type metal sulfide mercury removal agent price used in natural gas chemistry absorption hydrargyrum-removing technology is relatively low, de-
Mercury is efficient, is showed in moisture demercuration field superior.From economy, demercuration activity, accessibility angularly from the point of view of, metal vulcanization
The demercuration best performance of copper sulfide in object.Usually, the content of copper sulfide is higher in mercury removal agent, and demercuration efficiency is higher, to mercury
Adsorption capacity it is bigger, but the compression strength of mercury removal agent can reduce, and structural behaviour is poorer.Therefore, it is necessary to further increase negative
Carry copper sulfide demercuration activity, keep mercury removal agent identical in the load capacity of copper sulfide, obtain more preferably demercuration performance and
Structural behaviour.
Invention content
It is an object of the invention to solve above-mentioned problems of the prior art, a kind of height for moisture demercuration is provided
Imitate mercury removal agent.
Another object of the present invention is to provide a kind of preparation methods of the mercury removal agent for moisture demercuration.
For achieving the above object, the technical solution adopted in the present invention is：
A kind of mercury removal agent for moisture demercuration, the mercury removal agent include active material, carrier granular and auxiliary element；Institute
It is metal sulfide to state active material, mass fraction >=80% of copper sulfide in the active material；The carrier granular includes
Activated alumina, cocoanut active charcoal and adhesion promoter；The auxiliary element is silver sulfide；The quality of active material in the mercury removal agent
Score is 1~30%, and the mass fraction of activated alumina is 50~80%, and the mass fraction of cocoanut active charcoal is 5~30%, auxiliary
The mass fraction of co-ingredients is 0.05~5%；The active material and auxiliary element are supported in the carrier granular.
Preferably, the active material is copper sulfide.
Preferably, the mass fraction of active material is 10~25% in the mercury removal agent, the mass fraction of activated alumina
It is 50~70%, the mass fraction of cocoanut active charcoal is 10~30%, and the mass fraction of auxiliary element is 1~5%.
Preferably, the shape of the carrier granular is that spherical or tooth is spherical；A diameter of 1~10mm of the carrier granular；
The adhesion promoter is one or both of aluminous cement or palygorskite clay.
A kind of preparation method of the mercury removal agent for moisture demercuration, includes the following steps：
(1) activated alumina, cocoanut active charcoal and adhesion promoter are mixed, deionized water is added, after extrusion forming, drying
Carrier granular is made；
(2) carrier granular is impregnated into containing Cu2+And Ag+Solution in 3~5h, dipping completely after by the dipping
Carrier granular, which is placed at 500~800 DEG C, calcines the obtained mercury removal agent precursors of 1~2h；
(3) the mercury removal agent precursor is impregnated into 2~4h in sulfide solution to vulcanize, before the mercury removal agent after vulcanization
Body is placed in 1~2h of calcining at 500~800 DEG C, and mercury removal agent is made.
Preferably, the mass ratio of activated alumina, cocoanut active charcoal and adhesion promoter described in step (1) is 20:3:1~
16:7:1。
Preferably, drying described in step (1) is dry 3~4h at 80 DEG C；The shape of the carrier granular is spherical shape
Or tooth is spherical, a diameter of 1~10mm.
Preferably, Cu is contained described in step (2)2+And Ag+Solution be copper chloride or copper sulphate and silver nitrate mixing it is molten
Liquid；Cu in the mixed solution2+A concentration of 0.1~0.26mol/L, Ag+A concentration of 0.008~0.04mol/L；The load
Body particle contains Cu with described2+And Ag+Solution ratio be 55~80g/L.
Preferably, Cu is contained described in step (2)2+And Ag+Solution be copper carbonate or basic copper carbonate and silver nitrate ammonia
Aqueous solution；Cu in the solution2+A concentration of 0.1~0.26mol/L, Ag+A concentration of 0.008~0.04mol/L；The load
Body particle contains Cu with described2+And Ag+Solution ratio be 55~80g/L.
Preferably, sulfide solution described in step (3) is vulcanized sodium, potassium sulfide or ammonium sulfide solution；The sulfide
A concentration of 0.15~0.31mol/L of solution；The ratio of the mercury removal agent precursor and sulfide solution is 60~90g/L.
The beneficial effects of the invention are as follows：Provided by the present invention for moisture demercuration mercury removal agent carrier granular by active oxygen
Change aluminium and cocoanut active charcoal is prepared, can be used not only for moisture demercuration, also improve the adsorption capacity to organic mercury；It is described de-
Auxiliary element silver sulfide is added in mercurial, copper enhances the activity of active material copper sulfide with silver-colored synergistic effect, makes described
Mercury removal agent is identical in copper sulfide load capacity, obtains better demercuration performance；Provided by the present invention for moisture demercuration
Mercury removal agent preparation method using sulfide solution realize presoma mantoquita vulcanization, sulfidation endanger small, preparation process
Simply；In the Cu2+Ag is added in solution+, Ag+The strong interaction of aluminium oxide and active copper is reduced, forerunner can be promoted
The sulfurization of body mantoquita vulcanizes the silver sulfide of formation, can enhance the demercuration activity of active material copper sulfide, improve mercury removal agent
Demercuration performance.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear
Chu is fully described by, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without creative efforts
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
The preparation method of mercury removal agent for moisture demercuration includes the following steps：
(1) 100g activated aluminas and 20g cocoanut active charcoals are sufficiently mixed, 5g aluminous cements is added, be added appropriate
Distilled water, the spherical particle of a diameter of 3mm is then made of nodulizer extruding mixture, by manufactured spherical particle at 80 DEG C
Alumina carrier particle, specific surface area 238.2m are obtained after lower dry 4h2/ g, total pore volume 0.50cm3/g。
(2) 3.2g copper sulphate and 0.5g silver nitrates are dissolved in 100mL deionized waters, carrier granular described in 70g is impregnated
In above-mentioned mixed solution, dip time 4h；It is to be impregnated completely after, the carrier granular impregnated is calcined into 2h at 500 DEG C,
Mercury removal agent precursor is made.
(3) 2.3g vulcanized sodium is dissolved in 100mL deionized waters, the mercury removal agent precursor prepared is impregnated in above-mentioned vulcanization
Vulcanized in sodium solution, dip time 3h；It is to be impregnated completely after, the mercury removal agent precursor after vulcanization is calcined at 500 DEG C
2h obtains mercury removal agent finished product A.
Embodiment 2
The preparation method of mercury removal agent for moisture demercuration includes the following steps：
(1) 100g activated aluminas and 23g cocoanut active charcoals are sufficiently mixed, 5g aluminous cements is added, be added appropriate
Distilled water, the tooth spherical particle of a diameter of 3.8mm is then made of nodulizer extruding mixture, by manufactured tooth spherical particle
At 80 DEG C alumina carrier particle, specific surface area 213.5m are obtained after dry 5h2/ g, total pore volume 0.45cm3/g。
(2) 2.7g copper chlorides and 0.5g silver nitrates are dissolved in 100mL deionized waters, carrier granular described in 70g is impregnated
In above-mentioned mixed solution, dip time 5h；It is to be impregnated completely after, the carrier granular impregnated is calcined into 2h at 800 DEG C,
Mercury removal agent precursor is made.
(3) 3.3g potassium sulfides are dissolved in 100mL deionized waters, the mercury removal agent precursor prepared is impregnated in above-mentioned vulcanization
Vulcanized in potassium solution, dip time 4h；It is to be impregnated completely after, the mercury removal agent precursor after vulcanization is calcined at 800 DEG C
2h obtains mercury removal agent finished product B.
Embodiment 3
The preparation method of mercury removal agent for moisture demercuration includes the following steps：
(1) 100g activated aluminas and 25g cocoanut active charcoals are sufficiently mixed, 5g palygorskite clay is added, be added appropriate
Distilled water, the spherical particle of a diameter of 2.5mm is then made of nodulizer extruding mixture, by manufactured spherical particle 80
At DEG C alumina carrier particle, specific surface area 189.8m are obtained after dry 4h2/ g, total pore volume 0.40cm3/g。
(2) 3.3g copper carbonates and 0.6g silver nitrates are dissolved in 100mL ammonium hydroxide, on carrier granular is impregnated in described in 70g
It states in mixed solution, dip time 5h；It is to be impregnated completely after, carrier granular impregnate is calcined into 2h at 800 DEG C, it is obtained
Mercury removal agent precursor.
(3) 2.4g vulcanized sodium is dissolved in 100mL deionized waters, the mercury removal agent precursor prepared is impregnated in above-mentioned vulcanization
Vulcanized in sodium solution, dip time 5h；It is to be impregnated completely after, the mercury removal agent precursor after vulcanization is calcined at 800 DEG C
2h obtains mercury removal agent finished product C.
Comparative example
Preparation method described in this comparative example is as follows：
(1) 100g activated aluminas and 25g cocoanut active charcoals are sufficiently mixed, 5g palygorskite clay is added, be added appropriate
Distilled water, the spherical particle of a diameter of 2.5mm is then made of nodulizer extruding mixture, by manufactured spherical particle 80
At DEG C alumina carrier particle, specific surface area 189.8m are obtained after dry 4h2/ g, total pore volume 0.40cm3/g。
(2) 3.3g copper carbonates are dissolved in 100mL ammonium hydroxide, carrier granular described in 70g is impregnated in above-mentioned solution, impregnated
Time is 5h；It is to be impregnated completely after, carrier granular impregnate is calcined into 2h at 800 DEG C, obtained mercury removal agent precursor.
(3) 2.4g vulcanized sodium is dissolved in 100mL distilled water, the mercury removal agent precursor prepared is impregnated in above-mentioned vulcanized sodium
Vulcanized in solution, dip time 5h；It is to be impregnated completely after, the mercury removal agent precursor after vulcanization is calcined into 2h at 800 DEG C,
Obtain mercury removal agent finished product D.
Demercuration test is carried out respectively to mercury removal agent obtained in above-described embodiment 1-3 and comparative example, specific test behaviour
It is as condition：The mercury vapour that test gas is generated by high pure nitrogen and mercury vapour generator is mixed to get, and keeps first in gas
Beginning mercury content is 120 μ g/m3.ADSORPTION IN A FIXED BED reactor (organic glass adsorption column, internal diameter 20mm, mercury removal agent filling height
100mm, bed both ends use polytetrafluoroethylene (PTFE) paper to do supporting role instead of inert alumina porcelain ball) adsorption temp is environment temperature
Degree, pressure 0.5MPa, charge flow rate control test the mercury concentration in gas using the life of LUMEX companies of Russia in 0.15L/min
The RA-915+ mercury analyzers of production detect.
Mercury removal agent A-D is respectively charged into the experiment of ADSORPTION IN A FIXED BED reactor simulation natural gas mercury-removing, the test of each mercury removal agent
Time 240min is detected the mercury content in ADSORPTION IN A FIXED BED reactor outlet gas every 30min and (surveys 3 times, take it flat
Mean value), test result is as shown in table 1.
The demercuration test result of 1 mercury removal agent A-D of table
It can be seen from the test result of table 1 at normal temperatures demercuration when, mercury removal agent that 1-3 of the embodiment of the present invention is prepared
Show extremely strong adsorption capacity to the Elemental Mercury in gas phase, demercuration rate is up to 99% or more, even if the testing time reaches
240min still shows good stability.Mercury content in its exit gas of the mercury removal agent of the offer of embodiment 1 is 1.2~1.4
μg/m3, demercuration rate be slightly below embodiment 2 and 3 offer mercury removal agent, this be primarily due to embodiment 1 preparation mercury removal agent forge
It is 500 DEG C to burn temperature, and mercury removal agent calcination temperature prepared by embodiment 2 and 3 is 800 DEG C, shows calcination temperature to active material
Load capacity tool has a certain impact.Mercury content in its exit gas of the mercury removal agent of the offer of embodiment 2 is 0.1~0.2 μ g/m3,
Its demercuration effect is better than embodiment 3, this mercury removal agent particle for being primarily due to the preparation of embodiment 2 is that tooth is spherical, prepared by embodiment 3
Mercury removal agent particle be it is spherical, show that the shape of mercury removal agent influences its demercuration effect, the granularity of tooth spherical shape mercury removal agent will be slightly larger than
The granularity of spherical mercury removal agent, tooth spherical shape fine particle are closely packed together, and illustrate that Active components distribution is more uniform.
Mercury removal agent prepared by comparative example is not added with active auxiliary element sulphur compared with the mercury removal agent that embodiment 1-3 is provided
Change silver, the mercury content in exit gas is 20~23 μ g/m3, demercuration rate is only 80~83%, hence it is evident that is carried less than embodiment 1-3
The demercuration rate of the mercury removal agent of confession, this result shows that auxiliary element silver sulfide help to improve metal sulfide demercuration activity and
Mercury adsorption capacity.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features；
And these modifications or replacements, various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of mercury removal agent for moisture demercuration, which is characterized in that the mercury removal agent includes active material, carrier granular and auxiliary
Co-ingredients；The active material is metal sulfide, mass fraction >=80% of copper sulfide in the active material；The carrier
Particle includes activated alumina, cocoanut active charcoal and adhesion promoter；The auxiliary element is silver sulfide；Active matter in the mercury removal agent
The mass fraction of matter is 1~30%, and the mass fraction of activated alumina is 50~80%, and the mass fraction of cocoanut active charcoal is 5
~30%, the mass fraction of auxiliary element is 0.05~5%；The active material and auxiliary element are supported on the carrier granular
In.
2. a kind of mercury removal agent for moisture demercuration according to claim 1, which is characterized in that the active material is sulphur
Change copper.
3. a kind of mercury removal agent for moisture demercuration according to claim 1, which is characterized in that active in the mercury removal agent
The mass fraction of substance is 10~25%, and the mass fraction of activated alumina is 50~70%, the mass fraction of cocoanut active charcoal
It is 10~30%, the mass fraction of auxiliary element is 1~5%.
4. a kind of mercury removal agent for moisture demercuration according to claim 1, which is characterized in that the shape of the carrier granular
Shape is that spherical or tooth is spherical；A diameter of 1~10mm of the carrier granular；The adhesion promoter is that aluminous cement or palygorskite are viscous
One or both of soil.
5. a kind of preparation method of mercury removal agent such as Claims 1 to 4 any one of them for moisture demercuration, feature exist
In including the following steps：
(1) activated alumina, cocoanut active charcoal and adhesion promoter are mixed, deionized water is added, be made after extrusion forming, drying
Carrier granular；
(2) carrier granular is impregnated into containing Cu2+And Ag+Solution in 3~5h, dipping completely after by the carrier of the dipping
Particle, which is placed at 500~800 DEG C, calcines the obtained mercury removal agent precursors of 1~2h；
(3) the mercury removal agent precursor is impregnated into 2~4h in sulfide solution to vulcanize, the mercury removal agent precursor after vulcanization is set
1~2h is calcined at 500~800 DEG C, and mercury removal agent is made.
6. a kind of preparation method of mercury removal agent for moisture demercuration according to claim 5, which is characterized in that step
(1) mass ratio of activated alumina described in, cocoanut active charcoal and adhesion promoter is 20:3:1~16:7:1.
7. a kind of preparation method of mercury removal agent for moisture demercuration according to claim 5, which is characterized in that step
(1) drying described in is dry 3~4h at 80 DEG C；The shape of the carrier granular is that spherical or tooth is spherical, a diameter of 1~
10mm。
8. a kind of preparation method of mercury removal agent for moisture demercuration according to claim 5, which is characterized in that step
(2) contain Cu described in2+And Ag+Solution be copper chloride or copper sulphate and silver nitrate mixed solution；Cu in the mixed solution2+
A concentration of 0.1~0.26mol/L, Ag+A concentration of 0.008~0.04mol/L；The carrier granular contains Cu with described2+With
Ag+Solution ratio be 55~80g/L.
9. a kind of preparation method of mercury removal agent for moisture demercuration according to claim 5, which is characterized in that step
(2) contain Cu described in2+And Ag+Solution be copper carbonate or basic copper carbonate and silver nitrate ammonia spirit；Cu in the solution2+
A concentration of 0.1~0.26mol/L, Ag+A concentration of 0.008~0.04mol/L；The carrier granular contains Cu with described2+With
Ag+Solution ratio be 55~80g/L.
10. a kind of preparation method of mercury removal agent for moisture demercuration according to claim 5, which is characterized in that step
(3) sulfide solution described in is vulcanized sodium, potassium sulfide or ammonium sulfide solution；A concentration of the 0.15 of the sulfide solution~
0.31mol/L；The ratio of the mercury removal agent precursor and sulfide solution is 60~90g/L.
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| CN110343542A (en) * | 2019-04-23 | 2019-10-18 | 西南石油大学 | A kind of mercury removal agent and preparation method thereof for high mercurous liquid hydrocarbon demercuration |
| 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 |
| CN112191227A (en) * | 2020-10-12 | 2021-01-08 | 西南石油大学 | Mercury removing agent for natural gas and preparation method thereof |
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