CN108392941A - The preparation method of metal mercury absorbent, the adsorbent and regeneration method - Google Patents
The preparation method of metal mercury absorbent, the adsorbent and regeneration method Download PDFInfo
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- CN108392941A CN108392941A CN201810075213.9A CN201810075213A CN108392941A CN 108392941 A CN108392941 A CN 108392941A CN 201810075213 A CN201810075213 A CN 201810075213A CN 108392941 A CN108392941 A CN 108392941A
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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
- B01J20/0274—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
- B01J20/0296—Nitrates of compounds other than those provided for in B01J20/04
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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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
- B01J20/34—Regenerating or reactivating
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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
- B01J20/34—Regenerating or reactivating
- B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
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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
- B01J20/34—Regenerating or reactivating
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
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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
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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Abstract
The invention discloses a kind of preparation method of metal mercury absorbent, the regeneration methods of the adsorbent and the adsorbent, belong to chemisorption techniques field.The preparation method includes：Graphene oxide, the compound of at least one period 3 element, reducing agent are codissolved in ethanol solution, and are allowed to fully react, obtains the first intermediate product；Filtrate is made after filtering the first intermediate product；After filtrate is mixed with adhesive, successively after extrusion forming, drying for the first time, moulding material is obtained；After simultaneously being dried for the second time using the solution dip forming material of VI race's element, the second intermediate product is obtained；Second intermediate product is in CO2It is activated under atmosphere, activation temperature is 150 DEG C~200 DEG C, to which metal mercury absorbent be made.Meanwhile using certain regeneration method, the metal mercury absorbent being saturated is enabled to be regenerated.
Description
Technical field
The present invention relates to chemisorption techniques fields, more particularly to a kind of preparation method of metal mercury absorbent, the suction
Attached dose and regeneration method.
Background technology
With a large amount of burnings of fossil fuel, mercury pollution problem is increasingly severe.Wherein, the flue gas of coal fired power plant generation is
The important sources of mercury pollution.There are mainly three types of forms, including gaseous elemental mercury, bivalent mercury and particle for mercury in coal fired power plant flue gas
State mercury.Wherein：Bivalent mercury can be removed by desulfurizing tower, and particle mercury can be captured in deduster, and Elemental Mercury takes off
Except particularly difficult.
Currently, using gunite demercuration pressure can be brought to tail portion deduster, its performance is influenced.Though and fixed bed reactors
So can be to avoid the influence to tail portion deduster, but absorbent consumption is big, is not easy to regenerate, demercuration is of high cost.Using catalysis
When agent removes mercury, has to reaction temperature section and clearly limit.
Invention content
In view of this, the present invention provides a kind of preparation method of metal mercury absorbent, the adsorbent and the adsorbents to satisfy
Regeneration method with after has high demercuration efficiency, the mercury metal using the metal mercury absorbent that the preparation method is prepared
Adsorbent can still maintain higher demercuration efficiency after regeneration method regeneration, thus more suitable for application.
In order to reach above-mentioned first purpose, the technical solution of the preparation method of metal mercury absorbent provided by the invention is such as
Under：
The preparation method of metal mercury absorbent provided by the invention includes the following steps：
Graphene oxide, the compound of at least one period 3 element, reducing agent are codissolved in ethanol solution, and made
Abundant reaction, obtain the first intermediate product, wherein the matter of the compound of the graphene oxide and the period 3 element
The value range for measuring ratio is (95~83):(4~16)；
Filtrate is made after filtering first intermediate product；
After the filtrate is mixed with adhesive, successively after extrusion forming, drying for the first time, moulding material is obtained,
Wherein, the value range of the graphene oxide and the mass ratio of the binder is (1~20):(1~80)；
The solution of VI race's element is used to be obtained in second after impregnating the moulding material and second of drying as impregnating agent
Between product；
Second intermediate product is in CO2It is activated under atmosphere, activation temperature is 150 DEG C~200 DEG C；To which the gold be made
Belong to mercury absorbent.
The preparation method of metal mercury absorbent provided by the invention also can be used following technical measures and further realize.
Preferably, the graphene oxide is one or two kinds of in carboxylated graphene, amination graphene
Mixture.
Preferably, the compound of the period 3 element is selected from Al (NO3)3、Mg(NO3)2、Al2(SO4)3And MgSO4
At least one of.
Preferably, described adhesive is selected from Al2O3、SiO2、TiO2One or more of mixture.
Preferably, described adhesive is Al2O3。
Preferably, in the first time drying process, the value range of temperature is 80 DEG C~100 DEG C.
Preferably, in second of drying process, the value range of temperature is 100 DEG C~150 DEG C.
Preferably, the impregnating agent is Na2SeO4Solution, Na2SeO3Solution or Na2SeO4With Na2SeO3Mixing
Solution, and the value range of the mass percentage of solute is 5%~9%.
Preferably, second intermediate product is in CO2During being activated under atmosphere, activation temperature≤200 DEG C.
Preferably, in the reaction process for obtaining the first intermediate product, reactant is stirred.
Preferably, the mode of the stirring is mechanical agitation or magnetic agitation.
In order to reach above-mentioned second purpose, the technical solution of metal mercury absorbent provided by the invention is as follows：
Metal mercury absorbent provided by the invention is prepared into via the preparation method of metal mercury absorbent provided by the invention
It arrives.
In order to reach above-mentioned third purpose, the technology of the regeneration method after metal mercury absorbent saturation provided by the invention
Scheme is as follows：
Regeneration method after metal mercury absorbent saturation provided by the invention includes the following steps：
In N2The metal mercury absorbent of saturation is heated in atmosphere, the heating temperature is 200 DEG C~450
DEG C, the metal mercury absorbent after being regenerated.
It is further real that following technical measures also can be used in regeneration method after metal mercury absorbent saturation provided by the invention
It is existing.
Preferably, the heating temperature is 220 DEG C.
Preferably, in N2The cycle-index of the process heated to the metal mercury absorbent of the saturation in atmosphere is
5~8 times.
The advantageous effect of technical solution of the present invention is：The metal mercury absorbent being prepared using above-mentioned preparation method
Demercuration efficiency can reach 95% or more, by the demercuration efficiency energy for the regenerated metal mercury absorbent that above-mentioned regeneration method obtains
90% or more is enough maintained, commercial Application is more suitable for.
Description of the drawings
By reading the detailed description of hereafter preferred embodiment, various other advantages and benefit are common for this field
Technical staff will become clear.Attached drawing only for the purpose of illustrating preferred embodiments, and is not considered as to the present invention
Limitation.And throughout the drawings, the same reference numbers will be used to refer to the same parts.In the accompanying drawings：
Fig. 1 is the step flow chart of the preparation method of metal mercury absorbent provided in an embodiment of the present invention；
Fig. 2 illustrates for the variation relation of each substance in the preparation process of metal mercury absorbent provided in an embodiment of the present invention
Figure；
Fig. 3 be metal mercury absorbent provided in an embodiment of the present invention saturation after regeneration method during each substance variation
Relation schematic diagram.
Specific implementation mode
The present invention in order to solve the problems existing in the prior art, provides a kind of preparation method of metal mercury absorbent, the absorption
Agent and regeneration method using the metal mercury absorbent that the preparation method is prepared there is high demercuration efficiency, the mercury metal to inhale
Attached dose can still maintain higher demercuration efficiency after regeneration method regeneration, thus more suitable for application.
It is of the invention to reach the technological means and effect that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, to the preparation method of the metal mercury absorbent proposed according to the present invention, the adsorbent and the adsorbent
Regeneration method after saturation, specific implementation mode, structure, feature and its effect are described in detail as after.In the following description,
What different " embodiment " or " embodiment " referred to is not necessarily the same embodiment.In addition, feature in one or more embodiments,
Structure or feature can be combined by any suitable form.
The terms "and/or", only a kind of incidence relation of description affiliated partner, indicates that there may be three kinds of passes
System, for example, A and/or B, is specifically interpreted as：Can include A and B simultaneously, can be with individualism A, it can also individualism
B can have above-mentioned three kinds of any case.
Referring to attached drawing 1 and attached drawing 2, the preparation method for the metal mercury absorbent that the embodiment of the present invention one provides includes following step
Suddenly：
Step S1：Graphene oxide, the compound of at least one period 3 element, reducing agent are codissolved in ethanol solution
In, and be allowed to fully react, obtain the first intermediate product, wherein the matter of graphene oxide and the compound of period 3 element
The value range for measuring ratio is (95~83):(4~16)；
Step S2：Filtrate is made after filtering the first intermediate product；
Step S3：After filtrate is mixed with adhesive, successively after extrusion forming, drying for the first time, forming material is obtained
Material, wherein the value range of the mass ratio of graphene oxide and binder is (1~20):(1~80)；
Step S4：The solution of VI race's element is used to obtain second after dip forming material and for the second time drying as impregnating agent
Intermediate product；
Step S5：Second intermediate product is in CO2It is activated under atmosphere, activation temperature is 150 DEG C~200 DEG C；To which gold be made
Belong to mercury absorbent.
Wherein, one or two kinds of mixture of the graphene oxide in carboxylated graphene, amination graphene.
Wherein, the compound of period 3 element is selected from Al (NO3)3、Mg(NO3)2、Al2(SO4)3And MgSO4In at least
It is a kind of.
Wherein, adhesive is selected from Al2O3、SiO2、TiO2One or more of mixture.
Wherein, adhesive Al2O3。
Wherein, in first time drying process, the value range of temperature is 80 DEG C~100 DEG C.
Wherein, in second of drying process, the value range of temperature is 100 DEG C~150 DEG C.
Wherein, the impregnating agent of selection is Na2SeO4Solution, Na2SeO3Solution or Na2SeO4With Na2SeO3Mixing it is molten
The value range of liquid, the mass percentage of solute is 5%~9%.
Wherein, the second intermediate product is in CO2During being activated under atmosphere, activation temperature≤200 DEG C.
Wherein, in the reaction process for obtaining the first intermediate product, reactant is stirred.
Wherein, the mode of stirring is mechanical agitation or magnetic agitation, and higher porosity can be obtained using magnetic agitation.
As other embodiments, ethylene glycol or tetrahydrofuran also can be used in the solvent in step S1 in addition to ethanol solution
Solution.
Metal mercury absorbent provided by the invention is prepared into via the preparation method of metal mercury absorbent provided by the invention
It arrives.
Referring to attached drawing 3, the regeneration method after metal mercury absorbent saturation provided in an embodiment of the present invention includes the following steps：
In N2The metal mercury absorbent of saturation is heated in atmosphere, heating temperature is 200 DEG C~450 DEG C, is obtained again
Metal mercury absorbent after life.
Wherein, heating temperature is 220 DEG C.
Wherein, in N2During being heated to the metal mercury absorbent of saturation in atmosphere, heat cycles number be 5~
8 times.
According to technical solution described in the above embodiment, metal mercury absorbent of the present invention is prepared and regenerated at different conditions
Experimental data see the table below 1-1 and continued 1-2：
Table 1-1
Continued 1-2
In addition, being Mg (NO in period 3 element compound3)2、Al2(SO4)3、MgSO4Or mixed compound, or dipping
Agent is Na2SeO3Or Na2SeO4With Na2SeO3In the case of mixed solution, or use mechanical agitation, similar with 1 embodiment of table
Experiment condition under, regenerated under the demercuration efficiency and adsorbent difference cycle-index of the metal mercury absorbent of prepared acquisition
Demercuration efficiency afterwards, variation tendency is consistent with 1 data of table, so repeating no more.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (12)
1. a kind of preparation method of metal mercury absorbent, which is characterized in that include the following steps：
Graphene oxide, the compound of at least one period 3 element and reducing agent are codissolved in ethyl alcohol, ethylene glycol or tetrahydrochysene
It in tetrahydrofuran solution, and is allowed to fully react, obtains the first intermediate product, wherein the graphene oxide and the period 3
The value range of the mass ratio of the compound of element is (95~83):(4~16)；
Filtrate is made after filtering first intermediate product；
After the filtrate is mixed with adhesive, successively after extrusion forming, drying for the first time, moulding material is obtained, wherein
The value range of the graphene oxide and the mass ratio of the binder is (1~20):(1~80)；
The solution of VI race's element is used to obtain production among second after impregnating the moulding material and second of drying as impregnating agent
Object；
Second intermediate product is in CO2It is activated under atmosphere, activation temperature is 150 DEG C~200 DEG C；To which the mercury metal be made
Adsorbent.
2. the preparation method of metal mercury absorbent according to claim 1, which is characterized in that the graphene oxide is selected from
One or two kinds of mixture in carboxylated graphene, amination graphene.
3. the preparation method of metal mercury absorbent according to claim 1, which is characterized in that the period 3 element
Compound is selected from Al (NO3)3、Mg(NO3)2、Al2(SO4)3And MgSO4At least one of.
4. the preparation method of metal mercury absorbent according to claim 1, which is characterized in that described adhesive is selected from
Al2O3、SiO2、TiO2One or more of mixture.
5. the preparation method of metal mercury absorbent according to claim 4, which is characterized in that described adhesive Al2O3。
6. the preparation method of metal mercury absorbent according to claim 1, which is characterized in that the first time drying process
In, the value range of temperature is 80 DEG C~100 DEG C.
7. the preparation method of metal mercury absorbent according to claim 1, which is characterized in that second of drying process
In, the value range of temperature is 100 DEG C~150 DEG C.
8. the preparation method of metal mercury absorbent according to claim 1, which is characterized in that the impregnating agent is Na2SeO4
Solution, Na2SeO3Solution or Na2SeO4With Na2SeO3Mixed solution, and the value range of the mass percentage of solute
It is 5%~9%.
9. a kind of metal mercury absorbent, which is characterized in that be prepared via any method in claim 1~8.
10. a kind of regeneration method of metal mercury absorbent as claimed in claim 9, which is characterized in that include the following steps：
In N2The metal mercury absorbent of saturation is heated in atmosphere, the heating temperature is 200 DEG C~450 DEG C, is obtained
Metal mercury absorbent after regeneration.
11. the regeneration method of metal mercury absorbent according to claim 10, which is characterized in that the heating temperature is
220℃。
12. the regeneration method of metal mercury absorbent according to claim 10, which is characterized in that in the process of the heating
In, heat cycles number is 5~8 times.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110052243A (en) * | 2019-06-05 | 2019-07-26 | 遵义师范学院 | A kind of preparation method of the renewable mercury absorbent suitable for liquefied natural gas process |
| CN110314648A (en) * | 2019-07-02 | 2019-10-11 | 华北电力大学 | Preparation method, adsorbent and its regeneration method of nitrous oxide adsorbent |
| CN110496610A (en) * | 2019-08-28 | 2019-11-26 | 西安建筑科技大学 | A kind of regenerative agent and regeneration method for desulphurization denitration waste active carbon |
| CN110605108A (en) * | 2019-09-26 | 2019-12-24 | 西安建筑科技大学 | Method for regenerating desulfurization and denitrification waste active carbon |
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| CN110052243A (en) * | 2019-06-05 | 2019-07-26 | 遵义师范学院 | A kind of preparation method of the renewable mercury absorbent suitable for liquefied natural gas process |
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| CN110496610A (en) * | 2019-08-28 | 2019-11-26 | 西安建筑科技大学 | A kind of regenerative agent and regeneration method for desulphurization denitration waste active carbon |
| CN110605108A (en) * | 2019-09-26 | 2019-12-24 | 西安建筑科技大学 | Method for regenerating desulfurization and denitrification waste active carbon |
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