CN109482144A - A kind of desulfurization removes the preparation method of carbon adsorbent - Google Patents
A kind of desulfurization removes the preparation method of carbon adsorbent Download PDFInfo
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- CN109482144A CN109482144A CN201811653248.2A CN201811653248A CN109482144A CN 109482144 A CN109482144 A CN 109482144A CN 201811653248 A CN201811653248 A CN 201811653248A CN 109482144 A CN109482144 A CN 109482144A
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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
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
- C10L3/102—Removal of contaminants of acid contaminants
- C10L3/103—Sulfur containing contaminants
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
- C10L3/102—Removal of contaminants of acid contaminants
- C10L3/104—Carbon dioxide
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
- C10L2290/542—Adsorption of impurities during preparation or upgrading of a fuel
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Abstract
The invention belongs to pulping and paper-making industry methane purification fields, and in particular to a kind of desulfurization removes the preparation method of carbon adsorbent, is mainly used for the desulfurization of pulping and papermaking effluent biological fuel gas except carbon.The present invention is raw material by preparation nanoscale iron oxide particles, micro/nano level Si-Al molecular sieve, nano-cellulose is added as secondary pore-foaming agent, it is uniformly mixed with basis materials such as cement, high-temperature roasting, prepared desulfurization has the micro-nano three-dimensional cellular structure of even compact except carbon adsorbent.The desulfurization of the micro/nano level prepared by this method adsorbs H except carbon adsorbent selectivity is high2S and CO2Capacity is big, while having the advantages that regeneration is easy, and while improving the purity of biological fuel gas, expands the application of biological fuel gas, realizes the efficient utilization of biogas.
Description
Technical field
The invention belongs to pulping and paper-making industry methane purification fields, and in particular to a kind of desulfurization removes the preparation side of carbon adsorbent
Method is mainly used for pulping and papermaking effluent biomass fuel desulfurization except carbon.
Background technique
By pulping and papermaking effluent biological fuel gas impurity generate biogas ingredient it is more more miscellaneous, containing methane,
Carbon dioxide, hydrogen sulfide, hydrogen, carbon monoxide, oxygen and nitrogen etc..Main component and concentration in not purified biogas: first
Alkane content accounts for about 50~70%, and carbon dioxide accounts for about 25~40%, and hydrogen sulfide accounts for about 0.2~1%, and nitrogen accounts for about 1%, vapor
Account for about 2%, the content of the gases such as oxygen and carbon monoxide is below 1%.Hydrogen sulfide generates sulfur dioxide pair in combustion
The harm of the body and environment of people is larger；Carbon dioxide has fire extinguishing fire retardation, using combustion heat release or using work by combustion as mesh
System in, the presence of carbon dioxide would generally reduce the utilization rate of the combustion heat, reduce flame temperature, lead to heat release or acting
Increased costs in the process.Therefore biogas should remove hydrogen sulfide and carbon dioxide in use.
Currently, there are many method of processing biogas desulfurization both at home and abroad, according to its faintly acid and strong reducing property, carrying out desulfurization can divide
For dry and wet.Dry method is the reproducibility and combustibility using hydrogen sulfide, carrys out desulfurization or straight with solid oxidizer or adsorbent
Burning is connect, including Claus method, iron oxide process, activated carbon method and Ka Taisuerfufa etc..Wet process presses the difference used in it
Desulfurizing agent is divided into liquid absorption method and absorbs two class of oxidizing process.Have in liquid absorption method using alkaline solution chemical absorption method and
Utilize the Physical Absorption method and physical chemistry absorption process of organic solvent.It absorbs oxidizing process and mainly utilizes various oxidants, catalysis
Agent carries out desulfurization.The advantages of dry desulfurization has process short, and device structure is simple, and gas purification degree is high, smooth operation, and it is extensive
The biogas desulfurization less applied to sulfur content.Except carbon is most important process in biogas purifying production process, routine is dry except carbon has
Method and wet process.Dry method has pressure swing adsorption method, temp.-change adsorptive process；Wet process divides Physical Absorption method and chemical absorption method, Physical Absorption method
There are high-pressure washing method, low-temp methanol method, propylene carbonate ester process etc..
The method that domestic and international desulfurization removes carbon in comparison with the present application, is primarily present following aspect deficiency: (1) current existing biogas
Desulfurization decarbonizing technology is derived from natural gas extraction and production technology, its main feature is that decarbonizing technology treating capacity is small, sulfur removal technology adapts to model
Enclose wideless, foreign gas content and pulping and paper-making industry produce gas and have larger difference, and desulfurization removes carbon single effect, while carrying out desulfurization
Except the low efficiency of carbon.(2) conventional wet desulphurization removes carbon and mostly uses organic solvent, has corrosiveness, recovery efficiency to equipment
It is low, cause secondary pollution, and higher cost.(3) the existing hydramine method directly applied in pulping and paper-making industry marsh gas purifying and
Sulfone amine method causes sorbent circulation service life in methane desulfurization decarbonizing technology shorter because of the purification process using petrochemical industry,
Desulfurization is poor except the regenerability of carbon adsorbent, reduces the recycling rate of waterused that desulfurization removes carbon adsorbent, improves adsorbent handling
With.
104162342 A of CN discloses a kind of compound ionic liquid desulfurization and decarburization agent and its preparation method and application, tool
The preparation step of body, which includes: (i), adds water to form solution, stirring quantitative alkyl diamine；(ii) quantitative lactic acid is placed in drop
Liquid funnel instills lactic acid dropwise in alkyl diamine solution, and the reaction was continued after dripping off；(iii) quantitative sulfamic acid is passed through
It is reacted Gu material mouth is added in the solution of (ii) by spoon, the compound ionic liquid solution of product sulfamic acid lactic acid alkyl diamine.The method
Used ionic liquid desulfurization is cumbersome except carbon adsorbent preparation and operating process, higher cost, and without specific regenerability, together
When desulfurization except carbon effect lower than the present invention.104560252 A of CN discloses a kind of preparation side of selexol process decarburizer
Method, specific desulfurization and decarburization material include: (a) alkyl chain alcohol amine (b) morpholine derivative, (c) triazine derivative.Desulfurization and decarburization
Each component is uniformly mixed and both may be used in agent.Desulfurization and decarburization adsorbent cost used by this method is higher, and regenerability is poor, causes big
Measure the waste of material.
104190363 A of CN discloses a kind of calcium base decarbonization, desulfuration agent and its method of modifying and application, specific steps packet
Include: (i) is crushed and calcining: lime stone being crushed into powder, is calcined at high temperature.(ii) leaching is mixed: by Alcohol amine type sulfamic acid ion
Liquid is added to step calcined product, stirring.(iii) dry and dry object tabletting granulating.The desulfurization removes the use of carbon adsorbent
The mixed leaching of ionic liquid, higher cost, adsorbent preparation process energy consumption is larger, while having very high want to adsorbent equipment and operation
It asks.
Therefore develop it is a kind of prepare conveniently, low pollution is high-efficient, the good desulfurization of reusability except carbon adsorbent have pole
Its important meaning.
Summary of the invention
The present invention is directed to paper-making effluent biological fuel gas feature, provides the preparation side that a kind of desulfurization removes carbon adsorbent
Method can carry out desulfurization except carbon using the adsorbent that the present invention obtains simultaneously, and capacity is big, and regeneration is easy.
A kind of desulfurization of the present invention removes the preparation method of carbon adsorbent, is after nanoscale iron oxide particles, crystallization
Si-Al molecular sieve is raw material, and secondary pore-foaming agent and cement are added thereto, is uniformly mixed, extrusion forming, high-temperature roasting, cooling,
It obtains micro/nano level regenerating desulfurization and removes carbon adsorbent.
The nanoscale iron oxide particles the preparation method comprises the following steps: with FeCl3·6H2O, sodium hydroxide, surfactant are
Raw material, guidance preparation nanoscale iron oxide particles.
Si-Al molecular sieve is by ethyl orthosilicate, aluminium isopropoxide, sodium hydroxide, cetyl trimethyl after the crystallization
Ammonium bromide, a pore-foaming agent, water are prepared into gel, and then crystallization, ageing obtain.
The specific steps are that:
(1) by FeCl3·6H2O is soluble in water, is heated to 50~60 DEG C, and sodium hydroxide is added, adds cetyl three
Methyl bromide ammonium, is stirred continuously, and 30~50min is reacted at 50~60 DEG C, and entire reaction process inert gas shielding is sunk
It forms sediment, externally-applied magnetic field separation is washed, and freeze-drying obtains nanoscale iron oxide particles；
(2) it by ethyl orthosilicate, is added in the aqueous solution containing cetyl trimethylammonium bromide and a pore-foaming agent,
It is stirred at room temperature uniformly, obtains solution I；Aluminium isopropoxide and sodium hydroxide is soluble in water, obtain solution II；Solution II is dropped evenly
It in solution I, stirs evenly, obtains gel；It by gained gel thermostatic crystallization, washs, freeze-drying, the sial point after obtaining crystallization
Son sieve；
(3) secondary pore-foaming agent, nanoscale iron oxide particles, Si-Al molecular sieve are uniformly mixed with cement, extrusion forming, it is high
Temperature roasting obtains micro/nano level regenerating desulfurization except carbon adsorbent after cooling.
In the present invention, by the Si-Al molecular sieve of the nanometer ferro oxide and micro/nano level that will prepare, with the bases such as cement
Body material uniformly mixes, and adds secondary pore-foaming agent, and high-temperature calcination is prepared into the three-dimensional structure with uniform and fine and close duct,
For paper-making effluent methane purification, while having the function of desulfurization except carbon.
In step (1), by quality ratio, FeCl3·6H2O: sodium hydroxide: cetyl trimethylammonium bromide=1:0.8:
0.2。
The partial size of nano oxidized iron particle prepared by the present invention is mainly distributed on 50~80nm, temperature in experimentation and
Reaction time can all influence the preparation of particle, and reaction temperature is too low, and the reaction time is too short, influence ferric oxide particles nucleus and form speed
Degree and the speed of growth so that grain diameter is too small influence desulfurization effect.Reaction temperature is excessively high, and the reaction time is too long, then makes
Standby particle is excessive, meanwhile, biggish particle is unevenly distributed due to surfactant, it may occur that aggregation, so that specific surface area
Smaller, efficient desulfurization process is low.
Step (2) mainly prepares Si-Al molecular sieve gel, and wherein the silica alumina ratio of Si-Al molecular sieve is an important parameter, this
Application preparation Si-Al molecular sieve be used for paper-making effluent methane purification, so select molecular sieve Si/Al ratio 1~4 it
Between, it is the important parameter for determining the efficiency except carbon adsorbent.In the range, molecular sieve is suitable for biogas except carbon sublimated, sial
Molecular sieve reduces the absorption to methane gas to the absorption property highest of carbon dioxide, and silica alumina ratio is too large or too small, all
The purifying that will affect biogas leads to carbon dioxide adsorption low efficiency, or even increases the absorption to methane gas, makes biogas purifying effect
Rate is not high.
In step (2), by quality ratio, ethyl orthosilicate: aluminium isopropoxide: sodium hydroxide: cetyl trimethyl bromination
Ammonium: nano micro crystal cellulose: water=1:0.5:1:0.3:0.01:4, Si/Al=1~4 of Si-Al molecular sieve, one time pore-foaming agent is received
Rice microcrystalline cellulose, the temperature of the thermostatic crystallization are 50~60 DEG C, when crystallization a length of 72~80h.Sial prepared by the present invention
Molecular sieve has porous structure, and macropore is mostly 40~60nm, and aperture is mostly 6~10nm, and molecular sieve particle is uniform-spherical, grain
Diameter concentrates on 2-4mm.Molecular sieve process is prepared, crystallization temperature is too low, and crystallization time is too short, and Si-Al molecular sieve crystal grain forms speed
Slowly, the speed of growth is slow, it is too small to also result in Si-Al molecular sieve particle formation particle, while pore-forming is too small, easily blocks.Reaction temperature
Excessively high, the reaction time is too long, causes zeolite crystal excessive, and specific surface area is small, reduces adsorption efficiency.It prepares with this condition
Molecular sieve, even aperture distribution is moderate, is not easy to plug while improving molecular sieve specific surface area, and then improve adsorption efficiency.
In step (3), the mixture of secondary pore-foaming agent nano micro crystal cellulose and polyethylene glycol, by quality ratio, nanometer
Grade ferric oxide particles: Si-Al molecular sieve: nano micro crystal cellulose: polyethylene glycol: cement: water=0.8~1:1:0.3~0.6:
0.3~0.5:2~2.5:1.5~2, preparation desulfurization is except in carbon adsorbent each component quality proportioning, ferric oxide particles and sial divide
The content of son sieve is added according to the number of components of pulping and paper-making biogas, the very few efficiency that can all directly affect desulfurization and remove carbon, mistake
It causes waste of material more, while reducing being rich in for methane and spending.The nano micro crystal cellulose and polyethylene glycol of addition are as secondary cause
Hole agent excessively will cause desulfurization except carbon adsorbent mechanical properties decrease, while desulfurization is except the effective component attachment effect of carbon adsorbent
Fruit is poor, reduces regenerability, and the very few pore-creating character that will affect adsorbent of pore-foaming agent and three-dimensional channel are easily blocked, and same reduce takes off
Sulphur removes the efficiency of carbon.The proportion of water and cement mainly plays adhesive effect, easily by adsorbent group of effective components synthesis type.
The temperature that step (3) high temperature bakes is 600~700 DEG C, and calcining time is 4~5h, under this temperature and time,
Cement solidification molding, secondary pore-foaming agent pore effect is best, is formed by three-dimensional micro-nano channel aperture and is suitble to, is suitable for desulfurization
Except the use of carbon adsorbent.The pressure of extrusion forming is not higher than 107Pascal.
Compared with prior art, the invention has the following advantages that the adsorbent that (1) present invention obtains contains nanoscale
Iron particle and Si-Al molecular sieve, respectively to H2S and CO2Selective absorbing degree is very big, by with the materials such as basis material and pore-foaming agent
Material uniformly mixing, can carry out desulfurization except carbon, while also avoiding the absorption to methane gas simultaneously, have highly selective.(2) originally
Material used by inventing all is conventional material, while adding the nano micro crystal cellulose and/or polyethylene glycol of natural degradable
As pore-foaming agent, three-dimensional open-framework of the desulfurization of preparation except carbon adsorbent with even compact, hole is coherent, and porosity is high,
Increase the area that adsorbent is contacted with gas, is conducive to gas and sufficiently adsorbs and purify, the capacity that biogas purifies in unit volume
Greatly.(3) desulfurization prepared by the present invention can be blown except carbon adsorbent is with novel micro nanometer rice channel design by heating desorption
Adsorbent is swept, regeneration treatment is carried out to adsorbent, and power of regeneration is good, guarantee methane gas is rich in degree.(4) present invention is made
Standby desulfurization removes carbon adsorbent, can according to the constituent of pulping and paper-making industry biogas complexity, reasonably add can desulfurization remove
The constituent of carbon, the technique requirement of Lai Shiying biogas purifying.Meanwhile prepared desulfurization is except carbon adsorbent is in the process used
It is middle to be added without other medicaments, effectively avoid corrosion equipment.
Specific embodiment
The preparation of ferric oxide nanometer particle: FeCl is taken3·6H2O mass is 10g, is dissolved in 50mL water, is heated to 50 DEG C, is added
8g sodium hydroxide adds 2g surfactant cetyl trimethylammonium bromide, is stirred continuously, reacts 30min at 55 DEG C,
Entire reaction process inert gas shielding, is precipitated, and externally-applied magnetic field separation is washed and is freeze-dried, obtains nano iron oxide
Particle.
The preparation of Si-Al molecular sieve: by 10g ethyl orthosilicate, be added to containing 2.5g cetyl trimethylammonium bromide,
In the 30g aqueous solution of 0.1g nano micro crystal cellulose, it is stirred at room temperature uniformly.3g aluminium isopropoxide and 10g sodium hydroxide are dissolved in 10g
In water, obtained mixed liquor is dropped evenly in above-mentioned teos solution, is stirred evenly, gel is obtained.Gained is coagulated
Glue is placed in sealing device, and 50 DEG C of thermostatic crystallization 72h take out washing freeze-drying, the Si-Al molecular sieve after obtaining crystallization.
Embodiment 1
1.1 desulfurization remove the preparation of carbon adsorbent
1.5g nano micro crystal cellulose is evenly spread in 7.5g water, then 1.5g polyethylene glycol is dissolved in dispersion liquid
It stirs evenly, the nano oxidized iron particle of 4g, 5g Si-Al molecular sieve and 10g cement is added into dispersion liquid, be stirred at room temperature uniformly.?
Pressure about 107Pascal is put into 660 DEG C of kiln roastings and is cooled to room temperature after calcining time is 4.6h after extrusion forming,
The regenerating desulfurization containing micro-nano channel is prepared into except carbon adsorbent.
1.2 desulfurization remove the measurement of carbon adsorbent power of regeneration
At 25 DEG C, the maximum adsorption of carbon dioxide and hydrogen sulfide is measured respectively using high-precision intelligent mass-synchrometer
Amount.Regeneration gas heating after preheated drying, purges adsorbent to 200 DEG C or so, and take away the adsorbate being desorbed.Lead to again
High-precision intelligent quality analyzer is crossed, measurement regenerates 1 carbon dioxide and the maximal absorptive capacity of hydrogen sulfide, and iterative cycles are total
Before measurement regeneration, the desulfurization after regeneration 1 time, 5 times, 20 times is except carbon adsorbent is to the adsorption efficiency of carbon dioxide and hydrogen sulfide.
Embodiment 2
2.1 desulfurization remove the preparation of carbon adsorbent
2g nano micro crystal cellulose is evenly spread in 8g water, then 2.5g polyethylene glycol is dissolved in dispersion liquid and is stirred
Uniformly, the nano oxidized iron particle of 4g, 5g Si-Al molecular sieve and 10g cement are added into dispersion liquid, is stirred at room temperature uniformly.In pressure
About 107Pascal is put into 680 DEG C of kiln roastings and is cooled to room temperature after calcining time is 4.5h, prepared after extrusion forming
Carbon adsorbent is removed at the regenerating desulfurization containing micro-nano channel.
2.2 desulfurization remove the measurement of carbon adsorbent power of regeneration
At 25 DEG C, the maximum adsorption of carbon dioxide and hydrogen sulfide is measured respectively using high-precision intelligent mass-synchrometer
Amount.Regeneration gas heating after preheated drying, purges adsorbent to 200 DEG C or so, and take away the adsorbate being desorbed.Lead to again
High-precision intelligent quality analyzer is crossed, measurement regenerates 1 carbon dioxide and the maximal absorptive capacity of hydrogen sulfide, and iterative cycles are total
Before measurement regeneration, the desulfurization after regeneration 1 time, 5 times, 20 times is except carbon adsorbent is to the adsorption efficiency of carbon dioxide and hydrogen sulfide.
Embodiment 3
3.1 desulfurization remove the preparation of carbon adsorbent
2.5g nano micro crystal cellulose is evenly spread in 8g water, then 2g polyethylene glycol is dissolved in dispersion liquid and is stirred
Uniformly, the nano oxidized iron particle of 4.5g, 5g Si-Al molecular sieve and 11.5g cement are added into dispersion liquid, is stirred at room temperature uniformly.?
Pressure about 107Pascal is put into 640 DEG C of kiln roastings and is cooled to room temperature after calcining time is 4.4h after extrusion forming,
The regenerating desulfurization containing micro-nano channel is prepared into except carbon adsorbent.
3.2 desulfurization remove the measurement of carbon adsorbent power of regeneration
At 25 DEG C, the maximum adsorption of carbon dioxide and hydrogen sulfide is measured respectively using high-precision intelligent mass-synchrometer
Amount.Regeneration gas heating after preheated drying, purges adsorbent to 200 DEG C or so, and take away the adsorbate being desorbed.Lead to again
High-precision intelligent quality analyzer is crossed, measurement regenerates 1 carbon dioxide and the maximal absorptive capacity of hydrogen sulfide, and iterative cycles are total
Before measurement regeneration, the desulfurization after regeneration 1 time, 5 times, 20 times is except carbon adsorbent is to the adsorption efficiency of carbon dioxide and hydrogen sulfide.
Embodiment 4
4.1 desulfurization remove the preparation of carbon adsorbent
3g nano micro crystal cellulose is evenly spread in 9.5g water, then 2.5g polyethylene glycol is dissolved in dispersion liquid and is stirred
It mixes uniformly, the nano oxidized iron particle of 5g, 5g Si-Al molecular sieve and 12.5g cement is added into dispersion liquid, be stirred at room temperature uniformly.?
Pressure about 107Pascal is put into 650 DEG C of kiln roastings and is cooled to room temperature after calcining time is 4.2h after extrusion forming,
The regenerating desulfurization containing micro-nano channel is prepared into except carbon adsorbent.
4.2 desulfurization remove the measurement of carbon adsorbent power of regeneration
At 25 DEG C, the maximum adsorption of carbon dioxide and hydrogen sulfide is measured respectively using high-precision intelligent mass-synchrometer
Amount.Regeneration gas heating after preheated drying, purges adsorbent to 200 DEG C or so, and take away the adsorbate being desorbed.Lead to again
High-precision intelligent quality analyzer is crossed, measurement regenerates 1 carbon dioxide and the maximal absorptive capacity of hydrogen sulfide, and iterative cycles are total
Before measurement regeneration, the desulfurization after regeneration 1 time, 5 times, 20 times is except carbon adsorbent is to the adsorption efficiency of carbon dioxide and hydrogen sulfide.
Embodiment 5
5.1 desulfurization remove the preparation of carbon adsorbent
3g nano micro crystal cellulose is evenly spread in 10g water, then 2.5g polyethylene glycol is dissolved in dispersion liquid and is stirred
It mixes uniformly, the nano oxidized iron particle of 4g, 5g Si-Al molecular sieve and 12.5g cement is added into dispersion liquid, be stirred at room temperature uniformly.?
Pressure about 107Pascal is put into 700 DEG C of kiln roastings and is cooled to room temperature after calcining time is 4h, made after extrusion forming
It is standby to remove carbon adsorbent at the regenerating desulfurization containing micro-nano channel.
5.2 desulfurization remove the measurement of carbon adsorbent power of regeneration
At 25 DEG C, the maximum adsorption of carbon dioxide and hydrogen sulfide is measured respectively using high-precision intelligent mass-synchrometer
Amount.Regeneration gas heating after preheated drying, purges adsorbent to 200 DEG C or so, and take away the adsorbate being desorbed.Lead to again
High-precision intelligent quality analyzer is crossed, measurement regenerates 1 carbon dioxide and the maximal absorptive capacity of hydrogen sulfide, and iterative cycles are total
Before measurement regeneration, the desulfurization after regeneration 1 time, 5 times, 20 times is except carbon adsorbent is to the adsorption efficiency of carbon dioxide and hydrogen sulfide.
Embodiment 6
6.1 desulfurization remove the preparation of carbon adsorbent
3g nano micro crystal cellulose is evenly spread in 8.5g water, then 2.5g polyethylene glycol is dissolved in dispersion liquid and is stirred
It mixes uniformly, the nano oxidized iron particle of 4.5g, 5g Si-Al molecular sieve and 11.5g cement is added into dispersion liquid, be stirred at room temperature uniformly.
In pressure about 107Pascal is put into 680 DEG C of kiln roastings and is cooled to room after calcining time is 4.3h after extrusion forming
Temperature is prepared into the regenerating desulfurization containing micro-nano channel except carbon adsorbent.
6.2 desulfurization remove the measurement of carbon adsorbent power of regeneration
At 25 DEG C, the maximum adsorption of carbon dioxide and hydrogen sulfide is measured respectively using high-precision intelligent mass-synchrometer
Amount.Regeneration gas heating after preheated drying, purges adsorbent to 200 DEG C or so, and take away the adsorbate being desorbed.Lead to again
High-precision intelligent quality analyzer is crossed, measurement regenerates 1 carbon dioxide and the maximal absorptive capacity of hydrogen sulfide, and iterative cycles are total
Before measurement regeneration, the desulfurization after regeneration 1 time, 5 times, 20 times is except carbon adsorbent is to the adsorption efficiency of carbon dioxide and hydrogen sulfide.
Embodiment 7
7.1 desulfurization remove the preparation of carbon adsorbent
3g nano micro crystal cellulose is evenly spread in 9g water, then 1.5g polyethylene glycol is dissolved in dispersion liquid and is stirred
Uniformly, the nano oxidized iron particle of 5g, 5g Si-Al molecular sieve and 12g cement are added into dispersion liquid, is stirred at room temperature uniformly.In pressure
About 107Pascal is put into 650 DEG C of kiln roastings and is cooled to room temperature after calcining time is 4.2h, prepared after extrusion forming
Carbon adsorbent is removed at the regenerating desulfurization containing micro-nano channel.
7.2 desulfurization remove the measurement of carbon adsorbent power of regeneration
At 25 DEG C, the maximum adsorption of carbon dioxide and hydrogen sulfide is measured respectively using high-precision intelligent mass-synchrometer
Amount.Regeneration gas heating after preheated drying, purges adsorbent to 200 DEG C or so, and take away the adsorbate being desorbed.Lead to again
High-precision intelligent quality analyzer is crossed, measurement regenerates 1 carbon dioxide and the maximal absorptive capacity of hydrogen sulfide, and iterative cycles are total
Before measurement regeneration, the desulfurization after regeneration 1 time, 5 times, 20 times is except carbon adsorbent is to the adsorption efficiency of carbon dioxide and hydrogen sulfide.
Embodiment 8
8.1 desulfurization remove the preparation of carbon adsorbent
3g nano micro crystal cellulose is evenly spread in 10g water, then 2.5g polyethylene glycol is dissolved in dispersion liquid and is stirred
It mixes uniformly, the nano oxidized iron particle of 4g, 5g Si-Al molecular sieve and 12.5g cement is added into dispersion liquid, be stirred at room temperature uniformly.?
Pressure about 107Pascal is put into 690 DEG C of kiln roastings and is cooled to room temperature after calcining time is 4.5h after extrusion forming,
The regenerating desulfurization containing micro-nano channel is prepared into except carbon adsorbent.
8.2 desulfurization remove the measurement of carbon adsorbent power of regeneration
At 25 DEG C, the maximum adsorption of carbon dioxide and hydrogen sulfide is measured respectively using high-precision intelligent mass-synchrometer
Amount.Regeneration gas heating after preheated drying, purges adsorbent to 200 DEG C or so, and take away the adsorbate being desorbed.Lead to again
High-precision intelligent quality analyzer is crossed, measurement regenerates 1 carbon dioxide and the maximal absorptive capacity of hydrogen sulfide, and iterative cycles are total
Before measurement regeneration, the desulfurization after regeneration 1 time, 5 times, 20 times is except carbon adsorbent is to the adsorption efficiency of carbon dioxide and hydrogen sulfide.
Embodiment 9
9.1 remove the preparation of carbon adsorbent without containing the desulfurization of nano micro crystal cellulose and polyethylene glycol
The preparation of ferric oxide nanometer particle: FeCl is taken3·6H2O mass is 10g, is dissolved in 50mL water, is heated to 50 DEG C, is added
8g sodium hydroxide adds 2g surfactant cetyl trimethylammonium bromide, is stirred continuously, reacts 30min at 55 DEG C,
Entire reaction process inert gas shielding, is precipitated, and externally-applied magnetic field separation is washed and is freeze-dried, obtains nano iron oxide
Particle.
The preparation of Si-Al molecular sieve: by 10g ethyl orthosilicate, be added to containing 2.5g cetyl trimethylammonium bromide,
In 30g aqueous solution, it is stirred at room temperature uniformly.3g aluminium isopropoxide and 10g sodium hydroxide are dissolved in 10g water, the mixed liquor that will be obtained
It drops evenly in above-mentioned teos solution, stirs evenly, obtain gel.Gained gel is placed in sealing device, 50 DEG C
Thermostatic crystallization 72h takes out washing freeze-drying, the Si-Al molecular sieve after obtaining crystallization.
The nano oxidized iron particle of 4g, 5g Si-Al molecular sieve are distributed in 10g water.12.5g cement is added, is stirred at room temperature
It is even, in pressure about 107Pascal is put into 690 DEG C of kiln roastings and is cooled to after calcining time is 4.5h after extrusion forming
Room temperature.
9.2 desulfurization remove the measurement of carbon adsorbent power of regeneration
At 25 DEG C, the maximum adsorption of carbon dioxide and hydrogen sulfide is measured respectively using high-precision intelligent mass-synchrometer
Amount.Regeneration gas heating after preheated drying, purges adsorbent to 200 DEG C or so, and take away the adsorbate being desorbed.Lead to again
High-precision intelligent quality analyzer is crossed, measurement regenerates 1 carbon dioxide and the maximal absorptive capacity of hydrogen sulfide, and iterative cycles are total
Before measurement regeneration, the desulfurization after regeneration 1 time, 5 times, 20 times is except carbon adsorbent is to the adsorption efficiency of carbon dioxide and hydrogen sulfide.
Application example 1
It prepares desulfurization and removes carbon adsorbent, the ferric oxide particles of addition, Si-Al molecular sieve, nano micro crystal cellulose, poly- second two
The mass ratio of alcohol, cement and water is to add according to 0.8:1:0.3:0.3:2:1.5, adds the nanoscale iron oxide particles grain of preparation
Diameter is in 60~68nm, and the large aperture of Si-Al molecular sieve about 54~58nm, aperture is mostly 6~10nm, and partial size is in 2-3mm.Following table
For the measurement of power of regeneration:
Application example 2
It prepares desulfurization and removes carbon adsorbent, the ferric oxide particles of addition, Si-Al molecular sieve, nano micro crystal cellulose, poly- second two
The mass ratio of alcohol, cement and water is to add according to 0.8:1:0.4:0.5:2.2:1.6, adds the nanoscale iron oxide particles of preparation
Partial size is in 58~63nm, and the large aperture of Si-Al molecular sieve about 52~56nm, aperture is mostly 6~10nm, and partial size is in 2-3mm.Under
Table is the measurement of power of regeneration:
Application example 3
It prepares desulfurization and removes carbon adsorbent, the ferric oxide particles of addition, Si-Al molecular sieve, nano micro crystal cellulose, poly- second two
The mass ratio of alcohol, cement and water is to add according to 0.9:1:0.5:0.4:2.3:1.6, adds the nanoscale iron oxide particles of preparation
Partial size is in 62~68nm, and the large aperture of Si-Al molecular sieve about 55~59nm, aperture is mostly 6~10nm, and partial size is in 3-4mm.Under
Table is the measurement of power of regeneration:
Application example 4
It prepares desulfurization and removes carbon adsorbent, the ferric oxide particles of addition, Si-Al molecular sieve, nano micro crystal cellulose, poly- second two
The mass ratio of alcohol, cement and water is to add according to 1:1:0.6:0.5:2.5:1.9, adds the nanoscale iron oxide particles grain of preparation
Diameter is in 62~68nm, and the large aperture of Si-Al molecular sieve about 54~56nm, aperture is mostly 6~10nm, and partial size is in 3-4mm.Following table
For the measurement of power of regeneration:
Application example 5
It prepares desulfurization and removes carbon adsorbent, the ferric oxide particles of addition, Si-Al molecular sieve, nano micro crystal cellulose, poly- second two
The mass ratio of alcohol, cement and water is to add according to 0.8:1:0.6:0.5:2.5:2, adds the nanoscale iron oxide particles grain of preparation
Diameter is in 56~60nm, and the large aperture of Si-Al molecular sieve about 52~55nm, aperture is mostly 6~10nm, and partial size is in 3-4mm.Following table
For the measurement of power of regeneration:
Application example 6
It prepares desulfurization and removes carbon adsorbent, the ferric oxide particles of addition, Si-Al molecular sieve, nano micro crystal cellulose, poly- second two
The mass ratio of alcohol, cement and water is to add according to 0.9:1:0.6:0.5:2.3:1.7, adds the nanoscale iron oxide particles of preparation
Partial size is in 63~70nm, and the large aperture of Si-Al molecular sieve about 42~46nm, aperture is mostly 6~10nm, and partial size is in 3-4mm.Under
Table is the measurement of power of regeneration:
Application example 7
It prepares desulfurization and removes carbon adsorbent, the ferric oxide particles of addition, Si-Al molecular sieve, nano micro crystal cellulose, poly- second two
The mass ratio of alcohol, cement and water is to add according to 1:1:0.6:0.3:2.4:1.8, adds the nanoscale iron oxide particles grain of preparation
Diameter is in 60~64nm, and the large aperture of Si-Al molecular sieve about 43~45nm, aperture is mostly 6~10nm, and partial size is in 2-3mm.Following table
For the measurement of power of regeneration:
Application example 8
It prepares desulfurization and removes carbon adsorbent, the ferric oxide particles of addition, Si-Al molecular sieve, nano micro crystal cellulose, poly- second two
The mass ratio of alcohol, cement and water is to add according to 0.8:1:0.6:0.5:2.5:2, adds the nanoscale iron oxide particles grain of preparation
Diameter is in 65~68nm, and the large aperture of Si-Al molecular sieve about 46~50nm, aperture is mostly 6~10nm, and partial size is in 2-3mm.Following table
For the measurement of power of regeneration:
Application example 9
Prepare desulfurization and remove carbon adsorbent, the ferric oxide particles of addition, Si-Al molecular sieve, cement and water mass ratio be according to
0.8:1:2.5:2 addition, adds the nanoscale iron oxide particles partial size of preparation in 65~68nm, the large aperture of Si-Al molecular sieve is big
About 100-150nm, aperture are mostly 20-40nm, and partial size is in 2-3mm.Following table is the measurement of power of regeneration:
Claims (10)
1. the preparation method that a kind of desulfurization removes carbon adsorbent, which is characterized in that with sial after nanoscale iron oxide particles, crystallization point
Son sieve is raw material, and secondary pore-foaming agent and cement are added thereto, is uniformly mixed, extrusion forming, high-temperature roasting, cooling, is obtained micro-
Nanoscale regenerating desulfurization removes carbon adsorbent.
2. the preparation method that a kind of desulfurization according to claim 1 removes carbon adsorbent, which is characterized in that the nanoscale
Ferric oxide particles the preparation method comprises the following steps: with FeCl3·6H2O, sodium hydroxide, surfactant are raw material, and guidance prepares nanoscale
Ferric oxide particles, by quality ratio, FeCl3·6H2O: sodium hydroxide: surfactant=1:0.8:0.2.
3. the preparation method that a kind of desulfurization according to claim 1 removes carbon adsorbent, which is characterized in that prepare nanoscale oxygen
The temperature for changing iron particle is 50~60 DEG C, and the reaction time is 30~50min, and cetyl trimethylammonium bromide is surface-active
Agent.
4. the preparation method that a kind of desulfurization according to claim 1 removes carbon adsorbent, which is characterized in that after the crystallization
Si-Al molecular sieve is by ethyl orthosilicate, aluminium isopropoxide, sodium hydroxide, cetyl trimethylammonium bromide, pore-foaming agent, a water
It is prepared into gel, then crystallization, ageing obtain；By quality ratio, ethyl orthosilicate: aluminium isopropoxide: sodium hydroxide: cetyl
Trimethylammonium bromide a: pore-foaming agent: water=1:0.5:1:0.3:0.01:4.
5. the preparation method that a kind of desulfurization according to claim 4 removes carbon adsorbent, which is characterized in that the primary cause
Hole agent is nano micro crystal cellulose.
6. the preparation method that a kind of desulfurization according to claim 4 removes carbon adsorbent, which is characterized in that the crystallization temperature
Degree is 50~60 DEG C, when crystallization a length of 72~80h.
7. the preparation method that a kind of desulfurization according to claim 1 removes carbon adsorbent, which is characterized in that the secondary cause
Hole agent is the mixture of nano micro crystal cellulose and polyethylene glycol.
8. the preparation method that a kind of desulfurization according to claim 7 removes carbon adsorbent, which is characterized in that by quality ratio,
Nanoscale iron oxide particles: Si-Al molecular sieve after crystallization: nano micro crystal cellulose: polyethylene glycol: cement: water=0.8~1:1:
0.3~0.6:0.3~0.5:2~2.5:1.5~2.
9. the preparation method that a kind of desulfurization according to claim 1 removes carbon adsorbent, which is characterized in that the high temperature bakes
Temperature be 600~700 DEG C, calcining time be 4~5h.
10. the preparation method that a kind of desulfurization according to claim 1 removes carbon adsorbent, which is characterized in that described to be squeezed into
The pressure of type is not higher than 107Pascal.
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