CN106582893A - Pretreatment method for active carbon carrier of low-temperature denitration catalyst - Google Patents
Pretreatment method for active carbon carrier of low-temperature denitration catalyst Download PDFInfo
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Abstract
The invention discloses a pretreatment method for an active carbon carrier of a low-temperature denitration catalyst, wherein the pretreatment method comprises the following steps: S1, carrying out drying pretreatment on activated carbon; S2, placing the activated carbon after the drying treatment in an activation furnace, and carrying out activation treatment; S3, fully mixing the active carbon after the pre-activation treatment with an acid solution, and carrying out pickling treatment; S4, flushing the activated carbon after the pickling treatment with deionized water to be neutral, carrying out drying treatment on the washed activated carbon, and thus obtaining the modified active carbon sample of the low-temperature denitration catalyst carrier. The activated carbon sample pretreated by the pretreatment method has the advantages of large specific surface area, more abundant pore structure and larger proportion of mesopores and micropores, and the number of nitrogen-containing and oxygen-containing functional groups on the surface is increased. In the subsequent process of preparation of the denitration catalyst, the effective load amount of an active component precursor is greatly improved, and the active component is more closely combined with the carrier.
Description
Technical field
The invention belongs to catalyst technical field, and in particular to a kind of pre- place of the absorbent charcoal carrier of low-temperature denitration catalyst
Reason method.
Background technology
Activated carbon is a kind of amorphous carbon with labyrinth, with flourishing pore structure and huge specific surface
Product, and active surface chemical property.Traditional vanadium titanium denitrating catalyst, can only be at 350 DEG C using titanium dioxide as carrier
Competence exertion denitration under hot conditionss above, and the catalyst prepared as carrier with activated carbon, then can be at 150 DEG C even
Lower temperature is issued to very high denitration efficiency, therefore has broad application prospects in low-temperature denitration field.
On the other hand, merchandise active carbon specific surface area is limited, and distribution of pores is uneven, and surface functional group not enough enriches, such as straight
Connecing and catalyst being prepared as carrier, effect is general.Accordingly, it would be desirable to be modified pretreatment to activated carbon so as to which physical and chemical performance enters
One step is lifted, and better meets the requirement as denitration catalyst carrier material.
The content of the invention
Present invention aim to address the problems referred to above, there is provided a kind of pretreatment of the absorbent charcoal carrier of low-temperature denitration catalyst
Method, the preprocess method are modified to absorbent charcoal carrier so as to which physical and chemical performance gets a promotion, and are urged so as to improve low-temperature denitration
The performance of agent.
To solve above-mentioned technical problem, the technical scheme is that：A kind of absorbent charcoal carrier of low-temperature denitration catalyst
Preprocess method, comprise the following steps：
S1：It is dried pretreatment：Under 100～110 DEG C of constant temperatures, process is dried to activated carbon, is dried to constant weight；
S2：Pre-activate process：The activated carbon that drying in step S1 is processed is placed in activation furnace, nitrogen in activation furnace, is passed through
Used as shielding gas, using vapor as activator, high-temperature activation processes 3～10h to gas, and the activated carbon after pre-activate is processed is protected
Deposit standby；
S3：Pickling processes：The activated carbon that Jing pre-activate in step S2 is processed and acid solution, by quality of activated carbon：Acid is molten
Liquid volume ratio is 1：2～8 ratio is sufficiently mixed, and under 40～90 DEG C of water bath conditions, reacts 1～8h, by pickling processes
Activated carbon afterwards is saved backup；
S4：Cleaning-drying process：With the activated carbon of Jing pickling processes in deionized water repeatedly rinsing step S3, until washing
Liquid is close to neutrality, and the activated carbon to washing under 100～110 DEG C of constant temperature is dried process, is dried to constant weight, is obtained
As the modified activated carbon sample of low-temperature denitration catalyst carrier.
In above-mentioned technical proposal, step S1 is dried the purpose of pretreatment and is easy for subsequent step pre-activate to activated carbon
In process, the steam vapour amount being passed through needed for accurately calculating, the treatment effect of precise control activated carbon pre-activate process, because commodity
Activated carbon has certain moisture content in itself.Inventor's research finds that actually adoptable theoretical temperatures scope can be 100 for baking temperature
Between～150 DEG C.Baking temperature is higher than 100 DEG C, effectively by the free water inside activated carbon and could combine water all removings,
On the other hand, due to being usually in electric drying oven with forced convection to be dried process using air, and activated carbon is relatively inflammable, because
This temperature again can not be too high.In addition drying time is related to baking temperature, specifically can be according to the actual experiment condition of production depending on,
In the present invention, preferred baking temperature is 100～110 DEG C, and drying time is 12～24h.If being carried out using vacuum drying oven
Dried, then relevant temperature can also improve.It is all under the guiding theory of the present invention, select this area conventional drying mode and ginseng
Other drying modes and parameter in number, fall within protection scope of the present invention.
In above-mentioned technical proposal, the step S2 pre-activate is processed, and specifically includes following steps：
S21：The activated carbon that drying in step S1 is processed is placed in activation furnace, nitrogen is passed through in activation furnace as protection
Gas, after activation furnace is warming up to 400～500 DEG C, 1～3h of constant temperature；
S22：After activation furnace is continuously heating to 700～800 DEG C, vapor is passed through as activator, 1～3h of constant temperature；
S23：After activation furnace is continuously heating to 900～1000 DEG C, after 1～3h of constant temperature, stopping is passed through vapor, natural cooling
To room temperature, the activated carbon after pre-activate is processed is saved backup.
It should be noted that carrying out activation processing, its main purpose to the pretreated activated carbon of drying in activation furnace
It is that pore-creating is carried out to activated carbon, enriches the pore structure of activated carbon, increase specific surface area, improves in catalyst preparation process, carry
Active component adsorbance in body.It is, up to above-mentioned purpose, to this invention takes above-mentioned three sections as described in step S21～S23 and rise
Warm formula activating treatment method：Mainly there is the secondary carbonization process of activated carbon in the constant temperature stage at 500 DEG C；Priming reaction is that heat release is anti-
Should, need temperature occur at 700～800 DEG C or so, therefore be passed through vapor in 700～800 DEG C of constant temperature zones to be activated；
It is deep activation process to be continuously heating to 900～1000 DEG C.Further, examined based on energy-conservation and activated carbon toleration these two aspects
Consider, heating rate is too slow, causes the heating-up time long, power consumption is too many；Heating rate is too fast, and activated carbon toleration is limited, may
Because being heated, inequality causes structural deterioration.Different vapor is passed through speed, and the Properties of Activated Carbon difference after activation processing is also very big,
In pre-activate process step, vapor intake is the most important governing factor in addition to temperature.Jing inventor studies for a long period of time
Explore, preferred heating rate is 3～10 DEG C/min, and the speed that is passed through of vapor is 200～2000ml/kgh.It is all in the present invention
Guiding theory under, using other the Conventional activation process sides for carrying out activation processing in this area using activation furnace to activated carbon
Formula, falls within protection scope of the present invention.
In above-mentioned technical proposal, the purpose of pickling processes is to destroy activated carbon surface and internal unstable pore structure, together
Shi Zengjia activated carbon surface nitrogen-containing functional groups, oxygen-containing functional group, so as to improve active adsorption amount of the active component on carrier and
Conjugation.It is that, up to above-mentioned purpose, the present invention preferably acid solutions carry out pickling processes for 10%～80%.Acid solution can be selected
With but be not limited in sulphuric acid, hydrochloric acid, nitric acid, hypochlorous acid, potassium permanganate acid solution or hydrogen peroxide one or more.It is all
Under the guiding theory of the present invention, using other acid solutions in conventional acid solution in this area, the protection model of the present invention is fallen within
Enclose.
In above-mentioned technical proposal, as the loading process of active component needs to carry out in neutral environment, it is therefore desirable to spend
The acid solution remained in inside activated carbon surface product is cleaned up by ionized water, it is to avoid affect active component load effect.
The invention has the beneficial effects as follows：The pretreatment side of the absorbent charcoal carrier of the low-temperature denitration catalyst that the present invention is provided
Method, step are simple, and process control is strong.The activated carbon sample of the Jing preprocess method pretreatment, specific surface area are big, pore structure
More enrich, middle micropore ratio is bigger, while its surface is nitrogenous, the substantial increase of oxygen-containing functional group quantity.Denitration is prepared follow-up
During catalyst, active component presoma payload amount is increased dramatically, and active component precoded vector combination degree is more
Closely.The denitrating catalyst prepared, its denitration efficiency can just reach more than 90% at 150 DEG C, than not pretreated activity
Denitrating catalyst improved efficiency more than 20% prepared by high-area carbon.Meanwhile, its adaptability to NO fluctuation of concentrations and to SO2It is anti-
Toxicity all improves to some extent.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention is done below in conjunction with specific embodiment
Further describe in detail：
In following each specific embodiment, the activated carbon of employing is with a batch of merchandise active carbon.Jing is of the invention
The preprocess method of offer carries out pretreated modified activated carbon sample, the experiment of subsequent authentication modified activated carbon properties of sample
In, i.e., to being tested using the denitrating catalyst prepared by modified activated carbon sample, in the preparation process of denitrating catalyst,
Active component, preparation technology and preparation flow that each embodiment is adopted etc. are identical.
In following each embodiment, the preparation technology of denitrating catalyst is comprised the following steps：100 parts of deionized waters are taken,
Active component presoma is added thereto to, after abundant dissolving under certain condition, reaction, active component precursor solution is made.It is living
Property component presoma, including at least a kind of following compound：Certain change of the elements such as vanadium, tungsten, manganese, ferrum, cerium, molybdenum, nickel, cobalt, copper
Compound.The mass fraction of active component presoma is 1%～20%.100 parts of absorbent charcoal carriers are taken, by above-mentioned active component forerunner
Liquid solution is sufficiently mixed therewith, is stood 24h and is sufficiently impregnated with.The activated carbon after 24h will be stood to take out, in vacuum drying oven
In, under the conditions of 100～150 DEG C, 12～24h of freeze-day with constant temperature is to constant weight.Dried activated carbon is placed in activation furnace, with nitrogen
For shielding gas, with 3～10 DEG C of ramps to 400～600 DEG C, 1～3h of constant temperature naturally cools to room temperature, and low-temperature denitration is obtained
Catalyst.
In the examples below that, the low-temperature denitration catalyst that embodiment one is prepared into example IV use Jing this
The preprocess method of bright offer carries out the absorbent charcoal carrier of pretreatment, and embodiment five as a comparison case, is used without pre- place
The absorbent charcoal carrier of reason.
It should be noted that the preparation technology of denitrating catalyst the innovative point and protection domain of the present invention are not belonging to, only
It is that the performance of modified activated carbon sample to prepare to adopting the preprocess method that provides of the present invention is preferably tested, and
Denitrating catalyst is prepared for further, during this area may also be employed, other conventional denitrating catalyst preparation methoies are prepared.
Embodiment one
S1：It is dried pretreatment：Under 110 DEG C of constant temperatures, process is dried to merchandise active carbon, 24h is to perseverance for drying
Weight；
S2：Pre-activate process：The activated carbon for taking drying process in step S1 is placed in activation furnace, and nitrogen is passed through in activation furnace
Gas as shielding gas, using vapor as carrying out pre-activate process, specially following steps under activator, hot conditionss：
S21：The activated carbon 1kg for taking drying process in step S1 is placed in activation furnace, and nitrogen conduct is passed through in activation furnace
Shielding gas, after activation furnace is warming up to 500 DEG C, constant temperature 2h；
S22：After activation furnace is continuously heating to 800 DEG C, vapor is passed through as activator, constant temperature 1h；
S23：After activation furnace is continuously heating to 900 DEG C, after constant temperature 3h, stopping is passed through vapor, naturally cools to room temperature, will
Activated carbon after pre-activate process is saved backup；
In step S21～S23, the heating rate of activation furnace is 5 DEG C/min, and the speed that is passed through of vapor is 500ml/h；
S3：Pickling processes：100 parts of the activated carbon of Jing pre-activate process in step S2 is taken, is 40% sulfuric acid solution with concentration,
By quality of activated carbon：Sulfuric acid solution volume ratio is 1：3 ratio is sufficiently mixed, and under 60 DEG C of water bath conditions, 4h is little for reaction
When, the activated carbon after pickling processes is saved backup；
S4：Cleaning-drying process：With the activated carbon of Jing pickling processes in deionized water repeatedly rinsing step S3, until washing
To neutrality, the activated carbon to washing under 110 DEG C of constant temperature is dried process to liquid, and drying 24h to constant weight is obtained as low
The modified activated carbon sample of warm denitration catalyst carrier.
With the obtained modified activated carbon sample of the present embodiment as carrier, carbon based denitration catalyst is prepared into.
Jing is tested, and is 700mg/Nm in NO concentration3, O2Content is 6%, air speed 10000h-1Under the conditions of, when 120 DEG C, which takes off
Nitre efficiency reaches 78%, and when 150 DEG C, denitration efficiency reaches 88%, and when 180 DEG C, denitration efficiency reaches 93%.
Embodiment two
S1：It is dried pretreatment：Under 110 DEG C of constant temperatures, process is dried to merchandise active carbon, 24h is to perseverance for drying
Weight；
S2：Pre-activate process：The activated carbon for taking drying process in step S1 is placed in activation furnace, and nitrogen is passed through in activation furnace
Gas as shielding gas, using vapor as carrying out pre-activate process, specially following steps under activator, hot conditionss：
S21：The activated carbon 1kg for taking drying process in step S1 is placed in activation furnace, and nitrogen conduct is passed through in activation furnace
Shielding gas, after activation furnace is warming up to 500 DEG C, constant temperature 2h；
S22：After activation furnace is continuously heating to 800 DEG C, vapor is passed through as activator, constant temperature 1h；
S23：After activation furnace is continuously heating to 900 DEG C, after constant temperature 3h, stopping is passed through vapor, naturally cools to room temperature, will
Activated carbon after pre-activate process is saved backup；
In step S21～S23, the heating rate of activation furnace is 5 DEG C/min, and the speed that is passed through of vapor is 1000ml/h；
S3：Pickling processes：100 parts of the activated carbon of Jing pre-activate process in step S2 is taken, is 30% salpeter solution with concentration,
By quality of activated carbon：Salpeter solution volume ratio is 1：2 ratio is sufficiently mixed, and under 80 DEG C of water bath conditions, 4h is little for reaction
When, the activated carbon after pickling processes is saved backup；
S4：Cleaning-drying process：With the activated carbon of Jing pickling processes in deionized water repeatedly rinsing step S3, until washing
Liquid is close to neutrality, and the activated carbon to washing under 110 DEG C of constant temperature is dried process, and 24h is to constant weight for drying, is made
For the modified activated carbon sample of low-temperature denitration catalyst carrier.
With the obtained modified activated carbon sample of the present embodiment as carrier, carbon based denitration catalyst is prepared into.
Jing is tested, and is 700mg/Nm in NO concentration3, O2Content is 6%, air speed 10000h-1Under the conditions of, when 120 DEG C, which takes off
Nitre efficiency reaches 80%, and when 150 DEG C, denitration efficiency reaches 91%, and when 180 DEG C, denitration efficiency reaches 95%.
Embodiment three
S1：It is dried pretreatment：Under 110 DEG C of constant temperatures, process is dried to merchandise active carbon, 24h is to perseverance for drying
Weight；
S2：Pre-activate process：The activated carbon for taking drying process in step S1 is placed in activation furnace, and nitrogen is passed through in activation furnace
Gas as shielding gas, using vapor as carrying out pre-activate process, specially following steps under activator, hot conditionss：
S21：The activated carbon 1kg for taking drying process in step S1 is placed in activation furnace, and nitrogen conduct is passed through in activation furnace
Shielding gas, after activation furnace is warming up to 500 DEG C, constant temperature 2h；
S22：After activation furnace is continuously heating to 750 DEG C, vapor is passed through as activator, constant temperature 1h；
S23：After activation furnace is continuously heating to 900 DEG C, after constant temperature 3h, stopping is passed through vapor, naturally cools to room temperature, will
Activated carbon after pre-activate process is saved backup；
In step S21～S23, the heating rate of activation furnace is 5 DEG C/min, and the speed that is passed through of vapor is 500ml/h；
S3：Pickling processes：100 parts of the activated carbon of Jing pre-activate process in step S2 is taken, is 30% salpeter solution with concentration,
By quality of activated carbon：Salpeter solution volume ratio is 1：3 ratio is sufficiently mixed, and under 60 DEG C of water bath conditions, 4h is little for reaction
When, the activated carbon after pickling processes is saved backup；
S4：Cleaning-drying process：With the activated carbon of Jing pickling processes in deionized water repeatedly rinsing step S3, until washing
Liquid is close to neutrality, and the activated carbon to washing under 110 DEG C of constant temperature is dried process, and 24h is to constant weight for drying, is made
For the modified activated carbon sample of low-temperature denitration catalyst carrier.
With the obtained modified activated carbon sample of the present embodiment as carrier, carbon based denitration catalyst is prepared into.
Jing is tested, and is 700mg/Nm in NO concentration3, O2Content is 6%, air speed 10000h-1Under the conditions of, when 120 DEG C, which takes off
Nitre efficiency reaches 76%, and when 150 DEG C, denitration efficiency reaches 88%, and when 180 DEG C, denitration efficiency reaches 94%.
Example IV
S1：It is dried pretreatment：Under 110 DEG C of constant temperatures, process is dried to merchandise active carbon, 24h is to perseverance for drying
Weight；
S2：Pre-activate process：The activated carbon for taking drying process in step S1 is placed in activation furnace, and nitrogen is passed through in activation furnace
Gas as shielding gas, using vapor as carrying out pre-activate process, specially following steps under activator, hot conditionss：
S21：The activated carbon 1kg for taking drying process in step S1 is placed in activation furnace, and nitrogen conduct is passed through in activation furnace
Shielding gas, after activation furnace is warming up to 500 DEG C, constant temperature 2h；
S22：After activation furnace is continuously heating to 750 DEG C, vapor is passed through as activator, constant temperature 1h；
S23：After activation furnace is continuously heating to 950 DEG C, after constant temperature 3h, stopping is passed through vapor, naturally cools to room temperature, will
Activated carbon after pre-activate process is saved backup；
In step S21～S23, the heating rate of activation furnace is 5 DEG C/min, and the speed that is passed through of vapor is 1500ml/h；
S3：Pickling processes：100 parts of the activated carbon of Jing pre-activate process in step S2 is taken, is 60% sulfuric acid solution with concentration,
By quality of activated carbon：Sulfuric acid solution volume ratio is 1：3 ratio is sufficiently mixed, and under 80 DEG C of water bath conditions, 4h is little for reaction
When, the activated carbon after pickling processes is saved backup；
S4：Cleaning-drying process：With the activated carbon of Jing pickling processes in deionized water repeatedly rinsing step S3, until washing
Liquid is close to neutrality, and the activated carbon to washing under 110 DEG C of constant temperature is dried process, and 24h is to constant weight for drying, is made
For the modified activated carbon sample of low-temperature denitration catalyst carrier.
With the obtained modified activated carbon sample of the present embodiment as carrier, carbon based denitration catalyst is prepared into.
Jing is tested, and is 700mg/Nm in NO concentration3, O2Content is 6%, air speed 10000h-1Under the conditions of, when 120 DEG C, which takes off
Nitre efficiency reaches 78%, and when 150 DEG C, denitration efficiency reaches 88%, and when 180 DEG C, denitration efficiency reaches 93%.
Embodiment five
With not pretreated merchandise active carbon sample as carrier, carbon based denitration catalyst is prepared into.
Jing is tested, and is 700mg/Nm in NO concentration3, O2Content is 6%, air speed 10000h-1Under the conditions of, when 120 DEG C, which takes off
Nitre efficiency is 54%, and when 150 DEG C, denitration efficiency is 61%, and when 180 DEG C, denitration efficiency is 72%.
One of ordinary skill in the art will be appreciated that embodiment described here is to aid in reader and understands this
Bright principle, it should be understood that protection scope of the present invention is not limited to such especially statement and embodiment.This area
It is each that those of ordinary skill can make various other without departing from essence of the invention according to these technologies enlightenment disclosed by the invention
Plant concrete deformation and combine, these deformations and combination are still within the scope of the present invention.
Claims (7)
1. a kind of preprocess method of the absorbent charcoal carrier of low-temperature denitration catalyst, it is characterised in that：Comprise the following steps：
S1：It is dried pretreatment：Under 100～110 DEG C of constant temperatures, process is dried to activated carbon, is dried to constant weight；
S2：Pre-activate process：The activated carbon that drying in step S1 is processed is placed in activation furnace, nitrogen work in activation furnace, is passed through
For shielding gas, using vapor as activator, high-temperature activation processes 3～10h, and the activated carbon after high-temperature activation is processed is preserved
It is standby；
S3：Pickling processes：The activated carbon that Jing pre-activate in step S2 is processed and acid solution, by quality of activated carbon：Acid solution body
Product is than being 1：2～8 ratio is sufficiently mixed, and under 40～90 DEG C of water bath conditions, reacts 1～8h, after pickling processes
Activated carbon is saved backup；
S4：Cleaning-drying process：With the activated carbon of Jing pickling processes in deionized water repeatedly rinsing step S3, until cleaning mixture connects
Near to neutrality, the activated carbon to washing under 100～110 DEG C of constant temperature is dried process, dries to constant weight, obtains conduct
The modified activated carbon sample of low-temperature denitration catalyst carrier.
2. the preprocess method of the absorbent charcoal carrier of low-temperature denitration catalyst according to claim 1, it is characterised in that：Institute
In stating step S2, pre-activate is processed, and specifically includes following steps：
S21：The activated carbon that drying in step S1 is processed is placed in activation furnace, nitrogen is passed through in activation furnace as shielding gas,
After activation furnace is warming up to 400～500 DEG C, 1～3h of constant temperature；
S22：After activation furnace is continuously heating to 700～800 DEG C, vapor is passed through as activator, 1～3h of constant temperature；
S23：After activation furnace is continuously heating to 900～1000 DEG C, after 1～3h of constant temperature, stopping is passed through vapor, often naturally cools to
Temperature, the activated carbon after pre-activate is processed are saved backup.
3. the preprocess method of the absorbent charcoal carrier of low-temperature denitration catalyst according to claim 2, it is characterised in that：Institute
State in step S21-～S23, the heating rate of activation furnace is 3～10 DEG C/min.
4. the preprocess method of the absorbent charcoal carrier of low-temperature denitration catalyst according to claim 2, it is characterised in that：Institute
State in step S21-～S23, the speed that is passed through of vapor is 200～2000ml/kgh.
5. the preprocess method according to the absorbent charcoal carrier of the arbitrary described low-temperature denitration catalyst of claim 1-4, its feature
It is：The acid solutions are 10%～80%.
6. the preprocess method according to the absorbent charcoal carrier of the arbitrary described low-temperature denitration catalyst of claim 1-4, its feature
It is：In step S1, drying time is 12～24h.
7. the preprocess method according to the absorbent charcoal carrier of the arbitrary described low-temperature denitration catalyst of claim 1-4, its feature
It is：In step S3, during acid solution is sulphuric acid, hydrochloric acid, nitric acid, hypochlorous acid, potassium permanganate acid solution or hydrogen peroxide
At least one.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114471458A (en) * | 2021-10-21 | 2022-05-13 | 北京清新环境技术股份有限公司 | Modified activated carbon and preparation method thereof |
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