CN106693905A - Mercury-removing adsorbent and preparation method thereof - Google Patents

Mercury-removing adsorbent and preparation method thereof Download PDF

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Publication number
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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parts
adsorbent
benzoic acid
mercury
geraniol
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不公告发明人
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Henan Times Cloud Communication Technology Co Ltd
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Henan Times Cloud Communication Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/02Separation 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid 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
    • B01J20/043Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

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

A kind of demercuration adsorbent and preparation method thereof
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.
CN201611250036.0A 2016-12-29 2016-12-29 Mercury-removing adsorbent and preparation method thereof Pending CN106693905A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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

Cited By (1)

* Cited by examiner, † Cited by third party
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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