CN106621783B - A kind of compound sulfur and mercury removing agent and preparation method thereof - Google Patents
A kind of compound sulfur and mercury removing agent and preparation method thereof Download PDFInfo
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- CN106621783B CN106621783B CN201611200900.6A CN201611200900A CN106621783B CN 106621783 B CN106621783 B CN 106621783B CN 201611200900 A CN201611200900 A CN 201611200900A CN 106621783 B CN106621783 B CN 106621783B
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
- B01D53/82—Solid phase processes with stationary reactants
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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
- B01D53/04—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 with stationary adsorbents
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/64—Heavy metals or compounds thereof, e.g. mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
- B01D2253/1124—Metal oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/20—Organic adsorbents
- B01D2253/204—Metal organic frameworks (MOF's)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/30—Physical properties of adsorbents
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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
- B01D2257/30—Sulfur compounds
-
- 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
-
- 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
Abstract
The present invention relates to desulfuration demercuration technical fields, especially a kind of compound sulfur and mercury removing agent and preparation method thereof, it carries out being configured to sulfur and mercury removing agent by potassium chromate, calcium manganate, cobalt oxide, ethylenediamine, pyrolusite, the sulfur and mercury removing agent is removed sulfur-bearing, the sulfureous in flue gas of mercury ingredient, mercury ingredient, and its removal efficiency has reached 93% or more, can effectively reduce sulphur, mercury component content in flue gas, and raw material is easy to get, preparation cost is lower, reduces flue gas desulfurizing and hydrargyrum-removing cost.
Description
Technical field
The present invention relates to desulfuration demercuration technical field, especially a kind of compound sulfur and mercury removing agent and preparation method thereof.
Background technique
Coal is the main energy resources in China；The discharge that coal burns along with exhaust gas, and in coal, containing a large amount of
Sulfide and mercury, mercury has severe toxicity, readily volatilized, in coal combustion process, is volatized into environment, causes along with flue gas
The pollution of atmospheric environment；Moreover, mercury can also cause to seriously affect to organism, especially destroy the metabolism of biological cell
Function；Sulfide will be entered in environment in coal combustion process in the form of sulfur dioxide gas, cause to contain in air
A large amount of sulfur dioxide, with the landing of rainwater, sulfur dioxide, oxygen and water form acid rain, drop to earth's surface, cause earth's surface agriculture
The damages such as crop, vegetation, industrial factories and miness, bring the influence of high degree to production and living, therefore, for coal burning and exhausting
The desulfuration demercuration of flue gas is processed into for necessity.
Currently, the processing technique for flue gas desulfurizing and hydrargyrum-removing is more, but most of using individual desulfurization or de-
Mercury inorganic agent carries out substep desulfuration demercuration, and it is longer not only to cause the desulfuration demercuration period, but also desulfuration demercuration higher cost；It is based on
This, occurs the processing method by desulfuration demercuration while progress, and the selection to desulfuration demercuration raw material again in the prior art, makes
The cost for obtaining its desulfuration demercuration reduces, and if number of patent application is 201610149557, using low-grade pyrolusite as raw material, makes
During it react with smoke contacts, realize the removing to sulfur dioxide in flue gas and mercury, reduction flue gas emission process two
The content of sulfur oxide, mercury etc., reduces costs；But sulfur dioxide removal rate can only be increased to by the processing method
70% or so, the removal efficiency of mercury is increased to 64% or so, so that still containing a large amount of sulfide composition and mercury in flue gas
Ingredient, after draining into environment, serious self detergent power for exceeding environment still will cause the dirt of the high degree of environment
Dye.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention provide a kind of compound sulfur and mercury removing agent and its
Preparation method.
It is achieved particular by following technical scheme:
A kind of compound sulfur and mercury removing agent, material composition are 20-30 parts of pyrolusite, 1-3 parts of potassium chromate, mangaic acid in parts by weight
0.2-1.8 parts of calcium, 0.1-0.7 parts of cobalt oxide, 1-5 parts of ethylenediamine.
The material composition is 25 parts of pyrolusite, 2 parts of potassium chromate, 1.3 parts of calcium manganate, cobalt oxide 0.5 in parts by weight
Part, 3 parts of ethylenediamine.
The pyrolusite is ground into 20-80 mesh powder after microwave radiation processing.
The microwave irradiation power is 80-170W, microwave irradiation time 3-50min.
The pyrolusite is to be heated to 300-600 DEG C after being ground into the particle of 8-15 mesh, add water, so that occurring
Hydro-thermalization reaction, dusting obtain pyrolusite powder.
Above-mentioned compound sulfur and mercury removing agent preparation method, comprising the following steps:
(1) potassium chromate, calcium manganate, cobalt oxide are uniformly mixed, add water, so that moisture content is 15-27%, in vacuum condition
Under, use temperature for 100-120 DEG C of processing 20-40min；
(2) pyrolusite is prepared into powder, and the material of step (1) is added in pyrolusite powder, and add water kneading at
Mud is prepared into the particle that diameter is 0.04-1.7mm, is placed under nitrogen existence condition, in 150-240 DEG C of processing 0.8- by mud
Ethylenediamine is added in 1.3h.
The step (1), (2), the potassium hydroxide or lithium hydroxide for being 3-7% containing mass concentration in water.
Above-mentioned compound sulfur and mercury removing agent, sulfur-bearing, mercury fume for treatment temperature for 60-180 DEG C.
In fixed bed reactors, sulfur and mercury removing agent is filled in smoke filtration bed, with flow velocity is 8- by flue gas
11L/min is passed through in fixed bed reactors, under the flow velocity, what the height of sulfur and mercury removing agent filling to react with smoke contacts
Time is 20-30min.
Compared with prior art, the technical effect of the invention is embodied in:
It carries out being configured to sulfur and mercury removing agent by potassium chromate, calcium manganate, cobalt oxide, ethylenediamine, pyrolusite, so that the desulfurization
Mercury removal agent can remove sulfur-bearing, the sulfureous in flue gas of mercury ingredient, mercury ingredient, and its removal efficiency has reached 93% or more, can
Sulphur, the mercury component content in flue gas are effectively reduced, and raw material is easy to get, preparation cost is lower, reduces flue gas desulfurizing and hydrargyrum-removing
Cost.
Heating treatment under the mixed vacuum condition of potassium chromate, calcium manganate, cobalt oxide especially during the preparation process, so that
Under the high temperature conditions, three kinds of ingredient interactions, so that effective component is activated；And the mixed material after activation is added to
In pyrolusite powder, the activity of effective component in pyrolusite is promoted to improve, and combined to addition kneading into mud, and prepare glomeration
After particle, ethylenediamine mixing is added, so that its spherical particles surface has obtained modification, improves the adsorption capacity of spherical particles,
It improves to the sulphur in flue gas.The removal efficiency of mercury ingredient.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed
Range is not only limited to made description.
In certain embodiments, compound sulfur and mercury removing agent, material composition are 20-30 parts of pyrolusite, chromic acid in parts by weight
1-3 parts of potassium, 0.2-1.8 parts of calcium manganate, 0.1-0.7 parts of cobalt oxide, 1-5 parts of ethylenediamine.
In certain embodiments, the material composition is 25 parts of pyrolusite, 2 parts of potassium chromate, calcium manganate in parts by weight
1.3 parts, 0.5 part of cobalt oxide, 3 parts of ethylenediamine.
In certain embodiments, the pyrolusite is ground into 20-80 mesh powder after microwave radiation processing.It mentions
The high activity of pyrolusite, improves desulfuration demercuration efficiency.
In certain embodiments, the microwave irradiation power is 80-170W, microwave irradiation time 3-50min.
In certain embodiments, the pyrolusite is to be heated to 300-600 after being ground into the particle of 8-15 mesh
DEG C, add water, so that hydro-thermalization reaction occurs, dusting obtains pyrolusite powder.Unactivated ingredient in pyrolusite is activated, is improved de-
Reactivity after the addition of sulphur mercury removal agent, improves removal efficiency, reduces cost.
In certain embodiments, compound sulfur and mercury removing agent preparation method, comprising the following steps:
(1) potassium chromate, calcium manganate, cobalt oxide are uniformly mixed, add water, so that moisture content is 15-27%, in vacuum condition
Under, use temperature for 100-120 DEG C of processing 20-40min；
(2) pyrolusite is prepared into powder, and the material of step (1) is added in pyrolusite powder, and add water kneading at
Mud is prepared into the particle that diameter is 0.04-1.7mm, is placed under nitrogen existence condition, in 150-240 DEG C of processing 0.8- by mud
Ethylenediamine is added in 1.3h.
In certain embodiments, the step (1), (2), in water containing the potassium hydroxide that mass concentration is 3-7% or
Lithium hydroxide.So that manganese ingredient in alkali metal refined manganese dioxide base sulfur and mercury removing agent, improves desulfuration demercuration rate.
During using above-mentioned compound sulfur and mercury removing agent processing flue gas, flue gas is preferably 60-180 DEG C of sulfur-bearing, contains
Mercury flue gas.
It specifically in carrying out flue gas desulfurizing and hydrargyrum-removing treatment process, is incited somebody to action in fixed bed reactors or fluidized-bed reactor
Sulfur and mercury removing agent is filled in smoke filtration bed, and flue gas is passed through fixed bed reactors or stream with flow velocity for 8-11L/min
In fluidized bed reactor, under the flow velocity, the height of sulfur and mercury removing agent filling makes the time reacted with smoke contacts be 20-
30min。
Embodiment 1
Compound sulfur and mercury removing agent, material composition are pyrolusite 20kg, potassium chromate 1kg, calcium manganate 0.2kg, oxygen by weight
Change cobalt 0.1kg, ethylenediamine 1kg.
Preparation method, comprising the following steps:
(1) potassium chromate, calcium manganate, cobalt oxide are uniformly mixed, add water, so that moisture content is 15%, under vacuum conditions,
Use temperature for 100 DEG C of processing 20min；
(2) pyrolusite is prepared into powder, and the material of step (1) is added in pyrolusite powder, and add water kneading at
Mud is prepared into the particle that diameter is 0.04mm, is placed under nitrogen existence condition, in 150 DEG C of processing 0.8h, second two is added by mud
Amine.
Above-mentioned sulfur and mercury removing agent is handled into flue gas according to following application mode: in fixed bed reactors, by desulfuration demercuration
Agent is filled in smoke filtration bed, and flue gas is passed through in fixed bed reactors with flow velocity for 8L/min, under the flow velocity, desulfurization
The height of mercury removal agent filling makes the time reacted with smoke contacts be 30min.
Detection is 97.5% to the sulfur removal rate in flue gas, and mercury removal rate is 94.3%.
Embodiment 2
Compound sulfur and mercury removing agent, material composition are pyrolusite 30kg, potassium chromate 3kg, calcium manganate 1.8kg, oxygen by weight
Change cobalt 0.7kg, ethylenediamine 5kg.
Preparation method, comprising the following steps:
(1) potassium chromate, calcium manganate, cobalt oxide are uniformly mixed, add water, so that moisture content is 27%, under vacuum conditions,
Use temperature for 120 DEG C of processing 40min；
(2) 80 mesh powders are ground by pyrolusite after microwave radiation processing, microwave irradiation power 170W is micro-
The wave radiation time is 50min, and the material of step (1) is added in pyrolusite powder, and adds water kneading at mud, and mud is prepared into
Diameter is the particle of 1.7mm, is placed under nitrogen existence condition, and in 240 DEG C of processing 1.3h, ethylenediamine is added.
Above-mentioned sulfur and mercury removing agent is handled into flue gas according to following application mode: in a fluidized bed reactor, by desulfuration demercuration
Agent is filled in smoke filtration bed, and flue gas is passed through in fluidized-bed reactor with flow velocity for 11L/min, under the flow velocity, is taken off
The height of sulphur mercury removal agent filling makes the time reacted with smoke contacts be 20min.
Detection is 98.4% to the sulfur removal rate in flue gas, and mercury removal rate is 95.1%.
Embodiment 3
Compound sulfur and mercury removing agent, material composition are pyrolusite 25kg, potassium chromate 2kg, calcium manganate 1.3kg, oxygen by weight
Change cobalt 0.5kg, ethylenediamine 3kg.
Preparation method, comprising the following steps:
(1) potassium chromate, calcium manganate, cobalt oxide are uniformly mixed, add water, so that moisture content is 19%, under vacuum conditions,
Use temperature for 110 DEG C of processing 30min；
(2) by pyrolusite after being ground into the particle of 13 mesh, 400 DEG C is heated to, water is added, so that it is anti-that hydro-thermalization occurs
It answers, dusting, obtains pyrolusite powder, and the material of step (1) is added in pyrolusite powder, and add water kneading at mud, by mud
It is prepared into the particle that diameter is 0.8mm, is placed under nitrogen existence condition, in 170 DEG C of processing 1.1h, ethylenediamine is added.
Above-mentioned sulfur and mercury removing agent is handled into flue gas according to following application mode: in fixed bed reactors, by desulfuration demercuration
Agent is filled in smoke filtration bed, and flue gas is passed through in fixed bed reactors with flow velocity for 10L/min, under the flow velocity, is taken off
The height of sulphur mercury removal agent filling makes the time reacted with smoke contacts be 25min.
Detection is 96.3% to the sulfur removal rate in flue gas, and mercury removal rate is 97.1%.
Embodiment 4
Compound sulfur and mercury removing agent, material composition are pyrolusite 20kg, potassium chromate 3kg, calcium manganate 0.6kg, oxygen by weight
Change cobalt 0.3kg, ethylenediamine 4kg.
Preparation method, comprising the following steps:
(1) potassium chromate, calcium manganate, cobalt oxide are uniformly mixed, add water, the hydroxide for being 3% containing mass concentration in water
Potassium under vacuum conditions, uses temperature for 100 DEG C of processing 30min so that moisture content is 27%；
(2) 60 mesh powders are ground by pyrolusite after microwave radiation processing, microwave irradiation power 130W is micro-
The wave radiation time is 20min, and the material of step (1) is added in pyrolusite powder, and adds water kneading at mud, contains matter in water
The potassium hydroxide that concentration is 5% is measured, mud is prepared into the particle that diameter is 1.1mm, is placed under nitrogen existence condition, at 150 DEG C
1.3h is handled, ethylenediamine is added.
Above-mentioned sulfur and mercury removing agent is handled into flue gas according to following application mode: in a fluidized bed reactor, by desulfuration demercuration
Agent is filled in smoke filtration bed, and flue gas is passed through in fluidized-bed reactor with flow velocity for 8L/min, under the flow velocity, desulfurization
The height of mercury removal agent filling makes the time reacted with smoke contacts be 30min.
Detection is 96.9% to the sulfur removal rate in flue gas, and mercury removal rate is 95.7%.
Embodiment 5
Compound sulfur and mercury removing agent, material composition are pyrolusite 20kg, potassium chromate 2kg, calcium manganate 0.9kg, oxygen by weight
Change cobalt 0.6kg, ethylenediamine 2kg.
Preparation method, comprising the following steps:
(1) potassium chromate, calcium manganate, cobalt oxide are uniformly mixed, add water, the hydroxide for being 7% containing mass concentration in water
Lithium under vacuum conditions, uses temperature for 120 DEG C of processing 20min so that moisture content is 24%；
(2) by pyrolusite after being ground into the particle of 15 mesh, 500 DEG C is heated to, water is added, so that it is anti-that hydro-thermalization occurs
It answers, dusting, obtains pyrolusite powder, and the material of step (1) is added in pyrolusite powder, and add water kneading at mud, by mud
It is prepared into the particle that diameter is 0.5mm, is placed under nitrogen existence condition, in 240 DEG C of processing 1.3h, ethylenediamine is added.
Above-mentioned sulfur and mercury removing agent is handled into flue gas according to following application mode: in a fluidized bed reactor, by desulfuration demercuration
Agent is filled in smoke filtration bed, and flue gas is passed through in fluidized-bed reactor with flow velocity for 9L/min, under the flow velocity, desulfurization
The height of mercury removal agent filling makes the time reacted with smoke contacts be 27min.
Detection is 98.7% to the sulfur removal rate in flue gas, and mercury removal rate is 97.6%.
For the invention sulfur and mercury removing agent after handling flue gas desulfurizing and hydrargyrum-removing, directlyed adopt warm water immersion
Filtrate condensing crystallizing can be obtained the manganese sulfate product that purity is 63.7% or more by processing, filtering.
Claims (8)
1. a kind of compound sulfur and mercury removing agent, which is characterized in that material composition is 20-30 parts of pyrolusite, potassium chromate in parts by weight
1-3 parts, 0.2-1.8 parts of calcium manganate, 0.1-0.7 parts of cobalt oxide, 1-5 parts of ethylenediamine；
The preparation method of the compound sulfur and mercury removing agent, comprising the following steps:
(1) potassium chromate, calcium manganate, cobalt oxide are uniformly mixed, add water, so that moisture content is 15-27%, under vacuum conditions,
Use temperature for 100-120 DEG C of processing 20-40min；
(2) pyrolusite is prepared into powder, and the material of step (1) is added in pyrolusite powder, and add water kneading at mud, it will
Mud is prepared into the particle that diameter is 0.04-1.7mm, is placed under nitrogen existence condition, in 150-240 DEG C of processing 0.8-1.3h, adds
Enter ethylenediamine.
2. compound sulfur and mercury removing agent as described in claim 1, which is characterized in that the material composition is soft in parts by weight
25 parts of manganese ore, 2 parts of potassium chromate, 1.3 parts of calcium manganate, 0.5 part of cobalt oxide, 3 parts of ethylenediamine.
3. compound sulfur and mercury removing agent as claimed in claim 1 or 2, which is characterized in that the pyrolusite passes through microwave radiation
After processing, it is ground into 20-80 mesh powder.
4. compound sulfur and mercury removing agent as claimed in claim 3, which is characterized in that the microwave irradiation power is 80-170W,
Microwave irradiation time is 3-50min.
5. compound sulfur and mercury removing agent as claimed in claim 3, which is characterized in that the pyrolusite is by being ground into 8-15
After purpose particle, it is heated to 300-600 DEG C, adds water, so that hydro-thermalization reaction occurs, dusting obtains pyrolusite powder.
6. compound sulfur and mercury removing agent as described in claim 1, which is characterized in that the step (1), (2) contain matter in water
Measure the potassium hydroxide or lithium hydroxide that concentration is 3-7%.
7. compound sulfur and mercury removing agent as claimed in claim 1 or 2, sulfur-bearing, mercurous cigarette for treatment temperature for 60-180 DEG C
Gas.
8. compound sulfur and mercury removing agent application as claimed in claim 7, which is characterized in that in fixed bed reactors, by desulfurization
Mercury removal agent is filled in smoke filtration bed, flue gas is passed through in fixed bed reactors with flow velocity for 8-11L/min, in the flow velocity
Under, the height of sulfur and mercury removing agent filling makes the time reacted with smoke contacts be 20-30min.
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| CN103721556A (en) * | 2014-01-20 | 2014-04-16 | 高同柱 | Desulfurization, denitrification and demercuration additive as well as preparation method thereof |
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| CN103721556A (en) * | 2014-01-20 | 2014-04-16 | 高同柱 | Desulfurization, denitrification and demercuration additive as well as preparation method thereof |
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