CN106693905A - Mercury-removing adsorbent and preparation method thereof - Google Patents
Mercury-removing adsorbent and preparation method thereof Download PDFInfo
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- CN106693905A CN106693905A CN201611250036.0A CN201611250036A CN106693905A CN 106693905 A CN106693905 A CN 106693905A CN 201611250036 A CN201611250036 A CN 201611250036A CN 106693905 A CN106693905 A CN 106693905A
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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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- 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
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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Abstract
The invention discloses a mercury-removing adsorbent and a preparation method thereof. The adsorbent comprises the following raw materials in parts by weight: 29-37 parts of red jade soil, 1-5 parts of sodium hydrogen carbonate, 3-7 parts of geraniol and 11-19 parts of benzoic acid. The preparation method comprises the following steps: mixing and grinding the red jade soil and the sodium hydrogen carbonate, adding a benzoic acid solution, sealing, heating, stirring, dropwise adding the geraniol, cooling, performing ultrasonic treatment, performing microwave treatment, stirring till the solution is dry, and calcining at high temperature to obtain the adsorbent. The adsorbent prepared according to the preparation method provided by the invention greatly improves the mercury-removing efficiency, which reaches 95% or above, during flue gas mercury treatment through a synergistic effect of the raw materials, and is long in service life, environmentally friendly and free of secondary pollution; the preparation method is simple in process and short in process flow; the adsorbent is low in cost, is suitable for industrial production, can be reused after being used and calcined, can greatly reduce the mercury-removing cost and is suitable for large-scale application.
Description
Technical field
The present invention relates to atmosphere pollution technical field, specifically a kind of demercuration adsorbent and preparation method thereof.
Background technology
The mercury of Discharged form Coal Combustion is the main source of mercury pollution in air.Mercury in air can be by respiratory tract or food chain
Into human body, it is detrimental to health.Mercury pollution problem has become whole world focus of attention, is also China in the urgent need to address
Environmental problem.
Because the form of Mercury In Coal Combustion Flue Gas is based on Elemental Mercury, research both domestic and external is concentrated mainly on demercuration adsorbent
Develop.The more adsorbents of research have 5 kinds mostly at present：Activated carbon, flyash, Ca-base adsorbent, noble metal adsorbent, gold
Category oxide adsorbent and mineral substance adsorbent etc..Various adsorbents all existing defects in itself, although activated carbon have it is higher
Demercuration efficiency, but utilization rate is low.I.e. using utilization rate, corresponding cost meeting can be effectively improved after halide or sulfide removal
Continue to raise, be still difficult to heavy industrialization application, and activated carbon improper use may reduce flying dust can
Usability.Ca-base adsorbent is to Hg2+Adsorption efficiency it is higher, to Hg0Removal efficiency it is but very low.Noble metal and metal oxide
There is stronger selectivity to the absorption of mercury, while can be by Hg0It is oxidized to readily removed Hg2+, efficiency comparison is low.Mineral substance
The materials such as material, such as clay or zeolite, in China's rich reserves, are the very economic adsorbents of a class, but demercuration efficiency
It is relatively low.Although may be greatly improved by absorption property after modification, also without a kind of feasible processing means.Red beautiful soil
It is to be piled up to form by volcanic ash, is with a kind of widest soil media.Adsorption efficiency is low, but excellent with obvious price
How gesture, make its modified raising demercuration efficiency, is the problem that this patent need to be solved.
The content of the invention
It is an object of the invention to provide a kind of demercuration efficiency is high, long service life, non-secondary pollution, it is repeatable utilize,
Demercuration adsorbent of cost and preparation method thereof is greatly lowered, to solve the problems, such as to be proposed in above-mentioned background technology.
To achieve the above object, the present invention provides following technical scheme：
A kind of demercuration adsorbent, is made up of the following raw material according to weight portion：Red 29-37 parts of soil of jade, sodium acid carbonate 1-5 parts, perfume
Leaf-alcohol 3-7 parts, benzoic acid 11-19 parts.
As further scheme of the invention：The demercuration adsorbent, is made up of the following raw material according to weight portion：Red jade
It is native 31-35 parts, sodium acid carbonate 2-4 parts, geraniol 4-6 parts, benzoic acid 13-17 parts.
As further scheme of the invention：The demercuration adsorbent, is made up of the following raw material according to weight portion：Red jade
33 parts of soil, 3 parts of sodium acid carbonate, 5 parts of geraniol, 15 parts of benzoic acid.
Another object of the present invention is to provide a kind of preparation method of demercuration adsorbent, comprises the steps of：
1）8.5 times of ethanol of benzoic acid and its quality is mixed, benzoic acid solution is obtained；
2）By red beautiful soil and sodium acid carbonate mixed grinding, cross 120 mesh sieves, be subsequently adding benzoic acid solution, be warming up to 71 DEG C and
Stir process 1.6h is sealed at this temperature, 115 DEG C is then heated to and geraniol is added dropwise, stirred at such a temperature after being added dropwise to complete
18min, is then down to 68 DEG C and ultrasonically treated 37min, and ultrasonic power is 900W, then microwave treatment 12min, and microwave power is
1000W, then stirs to dry at a temperature of 99-101 DEG C, 3.9h is then calcined in 460 DEG C of Muffle furnace and obtains final product adsorbent.
Another object of the present invention is to provide application of the adsorbent in gas mercury treatment.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention by red beautiful soil and sodium acid carbonate mixed grinding, by obtained adsorbent, each original after benzoic acid, geraniol treatment
The synergy of material makes its demercuration efficiency be greatly improved, and reaches more than 95%, and long service life is more friendly to environment,
Non-secondary pollution.Present invention process is simple, technological process is short, with low cost, is suitable to industrialized production, after rear calcination processing
Can reuse, demercuration cost can be greatly lowered, be suitable to large-scale use.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of demercuration adsorbent is made up of the following raw material according to weight portion：Red beautiful soil 29 parts, carbonic acid
1 part of hydrogen sodium, 3 parts of geraniol, 11 parts of benzoic acid.
8.5 times of ethanol of benzoic acid and its quality is mixed, benzoic acid solution is obtained and is mixed red beautiful soil with sodium acid carbonate
Grind, cross 120 mesh sieves, be subsequently adding benzoic acid solution, be warming up to 71 DEG C and seal stir process 1.6h at such a temperature, then
It is warming up to 115 DEG C and geraniol is added dropwise, stir 18min after being added dropwise to complete at such a temperature, is then down to 68 DEG C and ultrasonically treated
37min, ultrasonic power is 900W, then microwave treatment 12min, and microwave power is 1000W, then stirred at a temperature of 99 DEG C to
It is dry, 3.9h is then calcined in 460 DEG C of Muffle furnace and obtains final product adsorbent.
Embodiment 2
In the embodiment of the present invention, a kind of demercuration adsorbent is made up of the following raw material according to weight portion：Red beautiful soil 37 parts, carbonic acid
5 parts of hydrogen sodium, 7 parts of geraniol, 19 parts of benzoic acid.
8.5 times of ethanol of benzoic acid and its quality is mixed, benzoic acid solution is obtained and is mixed red beautiful soil with sodium acid carbonate
Grind, cross 120 mesh sieves, be subsequently adding benzoic acid solution, be warming up to 71 DEG C and seal stir process 1.6h at such a temperature, then
It is warming up to 115 DEG C and geraniol is added dropwise, stir 18min after being added dropwise to complete at such a temperature, is then down to 68 DEG C and ultrasonically treated
37min, ultrasonic power is 900W, then microwave treatment 12min, and microwave power is 1000W, is then stirred at a temperature of 101 DEG C
To dry, 3.9h then calcined in 460 DEG C of Muffle furnace and obtains final product adsorbent.
Embodiment 3
In the embodiment of the present invention, a kind of demercuration adsorbent is made up of the following raw material according to weight portion：Red beautiful soil 31 parts, carbonic acid
2 parts of hydrogen sodium, 4 parts of geraniol, 13 parts of benzoic acid.
8.5 times of ethanol of benzoic acid and its quality is mixed, benzoic acid solution is obtained and is mixed red beautiful soil with sodium acid carbonate
Grind, cross 120 mesh sieves, be subsequently adding benzoic acid solution, be warming up to 71 DEG C and seal stir process 1.6h at such a temperature, then
It is warming up to 115 DEG C and geraniol is added dropwise, stir 18min after being added dropwise to complete at such a temperature, is then down to 68 DEG C and ultrasonically treated
37min, ultrasonic power is 900W, then microwave treatment 12min, and microwave power is 1000W, is then stirred at a temperature of 100 DEG C
To dry, 3.9h then calcined in 460 DEG C of Muffle furnace and obtains final product adsorbent.
Embodiment 4
In the embodiment of the present invention, a kind of demercuration adsorbent is made up of the following raw material according to weight portion：Red beautiful soil 35 parts, carbonic acid
4 parts of hydrogen sodium, 6 parts of geraniol, 17 parts of benzoic acid.
8.5 times of ethanol of benzoic acid and its quality is mixed, benzoic acid solution is obtained and is mixed red beautiful soil with sodium acid carbonate
Grind, cross 120 mesh sieves, be subsequently adding benzoic acid solution, be warming up to 71 DEG C and seal stir process 1.6h at such a temperature, then
It is warming up to 115 DEG C and geraniol is added dropwise, stir 18min after being added dropwise to complete at such a temperature, is then down to 68 DEG C and ultrasonically treated
37min, ultrasonic power is 900W, then microwave treatment 12min, and microwave power is 1000W, is then stirred at a temperature of 100 DEG C
To dry, 3.9h then calcined in 460 DEG C of Muffle furnace and obtains final product adsorbent.
Embodiment 5
In the embodiment of the present invention, a kind of demercuration adsorbent is made up of the following raw material according to weight portion：Red beautiful soil 33 parts, carbonic acid
3 parts of hydrogen sodium, 5 parts of geraniol, 15 parts of benzoic acid.
8.5 times of ethanol of benzoic acid and its quality is mixed, benzoic acid solution is obtained and is mixed red beautiful soil with sodium acid carbonate
Grind, cross 120 mesh sieves, be subsequently adding benzoic acid solution, be warming up to 71 DEG C and seal stir process 1.6h at such a temperature, then
It is warming up to 115 DEG C and geraniol is added dropwise, stir 18min after being added dropwise to complete at such a temperature, is then down to 68 DEG C and ultrasonically treated
37min, ultrasonic power is 900W, then microwave treatment 12min, and microwave power is 1000W, is then stirred at a temperature of 100 DEG C
To dry, 3.9h then calcined in 460 DEG C of Muffle furnace and obtains final product adsorbent.
Comparative example 1
In addition to sodium acid carbonate is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 2
In addition to benzoic acid is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 3
In addition to sodium acid carbonate and benzoic acid is not contained, its material content and preparation process are consistent with embodiment 5.
Embodiment 6
Demercuration treatment is carried out using the adsorbent obtained by above-described embodiment 1-5 and comparative example 1-3 point, as a result as shown in table 1.
The flue gas condition of experimental situation simulative power plant boiler, the Performance Test System of demercuration adsorbent is main by following part
Composition：Simulated flue gas produce part, simulated flue gas adapting device, heat-insulation system, adsorption reaction part, exhaust gas processing device.Mercury
Produced by osmos tube (permeability 175ng/min, VICI Metronics companies of the U.S. at room temperature), mercury emission is by water-bath crucible
Temperature control, use high-purity N2As carrier gas, SO is remixed2、O2And CO2, it is heated by gas mixer and attemperator
To actual flue-gas temperature scope, then by the fixed adsorption bed equipped with fly ash absorbent.Fixed reaction bed is a diameter of
150mm, is about the stainless steel cylinder of 300mm, additional asbestos heat-insulation layer.Reacted simulated flue gas are by after absorbent charcoal adsorber
Enter air, it is to avoid pollution is produced to air.During experiment, N is first passed through2, then adjust SO2、O2And CO2The flow of gas, gas
Total flow is controlled in about 20L/min.In this research, gas volume fraction is controlled to：0.2%SO2, 1%O2And 12%CO2, remaining is
N2, gas temperature is set to 150 DEG C.Mercuryvapour generator was demarcated for 25 DEG C before formal test in room temperature.By solid
Determine the mercury concentration before and after reaction bed to be measured by Zeemen effect analyzer (Russian RP-915+).According to reaction before and after mercury concentration come
Calculate the adsorption rate to mercury of adsorbent, i.e. η=(C0-C)/C0×100%.In formula, η represents the adsorption rate of mercury, %；C0Represent import
Gas mercury concentration, μ g/m3；C represents outlet gas mercury concentration, μ g/m3。
Table 1
| Mercury adsorption rate（%） | |
| Embodiment 1 | 95.8 |
| Embodiment 2 | 96.2 |
| Embodiment 3 | 98.5 |
| Embodiment 4 | 98.9 |
| Embodiment 5 | 99.6 |
| Comparative example 1 | 68.4 |
| Comparative example 2 | 41.3 |
| Comparative example 3 | 35.5 |
In all samples, the adsorbent of embodiment 5 has respectively reached 99.6% to the adsorption rate highest of Elemental Mercury.Other samples it is de-
Mercury efficiency is below the sample of embodiment 5.After embodiment 5 shows sodium acid carbonate and benzoic acid addition with the result of comparative example 1-3
The suction-operated of adsorbent can be greatly promoted.Therefore, sodium acid carbonate and benzoic acid and its addition influence on performance of the adsorbent
It is larger.From contrast experiment as can be seen that using the adsorbent that preparation method disclosed by the invention is prepared there is more preferable mercury to take off
Except rate, this is that those skilled in the art cannot predict, and achieves unexpected technique effect.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires to be limited rather than described above, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each implementation method is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Specification an as entirety, the technical scheme in each embodiment can also be formed into those skilled in the art through appropriately combined
May be appreciated other embodiment.
Claims (5)
1. a kind of demercuration adsorbent, it is characterised in that be made up of the following raw material according to weight portion：Red 29-37 parts of soil of jade, carbonic acid
1-5 parts, geraniol 3-7 parts, benzoic acid 11-19 parts of hydrogen sodium.
2. demercuration adsorbent according to claim 1, it is characterised in that be made up of the following raw material according to weight portion：It is red
Beautiful 31-35 parts, sodium acid carbonate 2-4 parts, geraniol 4-6 parts, benzoic acid 13-17 parts of soil.
3. demercuration adsorbent according to claim 1, it is characterised in that be made up of the following raw material according to weight portion：It is red
Beautiful 33 parts of soil, 3 parts of sodium acid carbonate, 5 parts of geraniol, 15 parts of benzoic acid.
4. the preparation method of a kind of demercuration adsorbent as described in claim 1-3 is any, it is characterised in that by following steps group
Into：
1）8.5 times of ethanol of benzoic acid and its quality is mixed, benzoic acid solution is obtained；
2）By red beautiful soil and sodium acid carbonate mixed grinding, cross 120 mesh sieves, be subsequently adding benzoic acid solution, be warming up to 71 DEG C and
Stir process 1.6h is sealed at this temperature, 115 DEG C is then heated to and geraniol is added dropwise, stirred at such a temperature after being added dropwise to complete
18min, is then down to 68 DEG C and ultrasonically treated 37min, and ultrasonic power is 900W, then microwave treatment 12min, and microwave power is
1000W, then stirs to dry at a temperature of 99-101 DEG C, 3.9h is then calcined in 460 DEG C of Muffle furnace and obtains final product adsorbent.
5. application of the adsorbent as described in claim 1-3 is any in gas mercury treatment.
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| CN201611250036.0A CN106693905A (en) | 2016-12-29 | 2016-12-29 | Mercury-removing adsorbent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003883A (en) * | 2017-11-15 | 2018-05-08 | 郑州源冉生物技术有限公司 | A kind of stabilizer for handling organic pollution of soil and its preparation method and application |
-
2016
- 2016-12-29 CN CN201611250036.0A patent/CN106693905A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003883A (en) * | 2017-11-15 | 2018-05-08 | 郑州源冉生物技术有限公司 | A kind of stabilizer for handling organic pollution of soil and its preparation method and application |
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