CN110127692A - A kind of preparation method of mesoporous heat-resistant activity charcoal - Google Patents
A kind of preparation method of mesoporous heat-resistant activity charcoal Download PDFInfo
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- CN110127692A CN110127692A CN201910438211.6A CN201910438211A CN110127692A CN 110127692 A CN110127692 A CN 110127692A CN 201910438211 A CN201910438211 A CN 201910438211A CN 110127692 A CN110127692 A CN 110127692A
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- activity charcoal
- resistant activity
- mesoporous
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
Abstract
The present invention relates to a kind of preparation methods of mesoporous heat-resistant activity charcoal.This method specifically has the following steps: step A: blocky coal tar pitch is clayed into power；Step B: coal tar pitch powder and magnesium oxide powder are uniformly mixed；Step C: mixing sample is fitted into corundum boat, corundum boat is put into tube furnace；Step D: above-mentioned sample is heated in nitrogen atmosphere；Step E: the Carbon Materials fired are clayed into power, and carry out pickling；Step F: the Carbon Materials after pickling are dried, and obtain powdery mesoporous heat-resistant activity charcoal；Step G: powdery mesoporous heat-resistant activity charcoal is granulated.The mesoporous heat-resistant activity charcoal has the advantage that preparation cost is low, and preparation process is simple, utilization easy to produce；Aperture is mesoporous, adsorbable organic gas, is also easy desorption；Pore size is adjustable；It is resistant to 400 DEG C of temperature.
Description
Technical field
The present invention relates to adsorb effective active carbon field, and in particular to a kind of preparation method of mesoporous heat-resistant activity charcoal.
Background technique
Active carbon is specific surface area usually in 80-1500m2The porous charcoal of/g, it being capable of dyestuff, metal in adsorbent solution
The pollutants such as ion, pigment can also adsorb the volatile organic compounds in air.Active carbon be frequently used in industrial production and
In daily life.
Volatile organic compounds (VOCs) are harmful to the human body, and in the higher situation of concentration, can cause nervous lesion, in lung
Poison, septicemia, liver kidney and metabolic system poisoning.The method of detection VOCs generallys use adsorption tube adsorption-desorption-
The method of analysis.Adsorption tube plays critically important role in analysis volatile organic compounds, and the filler in adsorption tube
It is the core of adsorption tube.These fillers generally use Tenax filler, and this material is mainly central hole structure, can be to having
Machine escaping gas is effectively adsorbed, and under conditions of heating air blowing, organic gas molecule again can be under Tenax material desorption
Come.Tenax material high temperature resistant, can be subjected to 400 DEG C of desorption temperature.But this material price is extremely expensive, 100g's sells
Valence often reaches tens of thousands of members, is unfavorable for promoting and use.
Therefore, this invention address that develop one kind have in, macroporous structure (10-100nm), heat-resist (can be subjected to
400 DEG C) and the cheap effective filling active carbon of absorption.
Summary of the invention
The present invention provides a kind of preparation method of mesoporous heat-resistant activity charcoal, including the following steps:
Step A: selecting at least one of selected from coal tar pitch and petroleum asphalt, coal tar or carbolineum to be used as carbon source, selects 80nm oxidation
At least one of magnesium, 50nm magnesia or light magnesium oxide are used as template；
Step B: with the mode of grinding by blocky coal tar pitch grinds shape, the powdery of 100 mesh of granularity < is filtered out with sieve
Coal tar pitch, adds 80nm magnesia, obtains mixing sample after mixing evenly, and mixing sample is put into corundum boat；
Step C: the corundum boat equipped with mixing sample is put into tube furnace, and heating mixing sample obtains in inert gas
Blocky carbon material, then cools to room temperature, and inert gas is nitrogen, nitrogen flow 30-40ml/min；
Step D: the blocky carbon material fired of heating is pulverized shape carbon material, powdery carbon material is put into glass and is burnt
In cup, hydrochloric acid is added according to 1.1-1.3 times of 80nm magnesia mole, selecting concentration is the hydrochloric acid of 1.5-2.5mol/L, is used
The mixed solution 22-26h of magnetic stirrer above-mentioned powdery carbon material and hydrochloric acid, the powdery carbon materials after pickling is obtained by filtration
Material, the powdery carbon material after pickling is placed again into clean glass beaker, and the distilled water that water temperature is 70-90 DEG C is added,
The volume of distilled water is the 2/3-4/5 of beaker capacity, stirs 5-10min, and be filtered, and the process of distillation washing carbon repeats 2-
3 times, the powdery carbon material after obtaining template；
Step E: being dried going the powdery carbon material after template to be put into drying box, and drying temperature is 100-110 DEG C,
Obtain dry powdery mesoporous heat-resistant activity charcoal；
Step F: powdery mesoporous heat-resistant activity charcoal, crosslinking agent and distilled water are mixed according to mass percent, stirred evenly
To paste, pasty mixture is obtained, and crosslinking agent selects lithium metasilicate magnesium；
Step G: pasty mixture is spread in corundum boat with spoon, keeps the thickness of pasty mixture uniform, and thickness
For 3-4cm, then hot briquetting obtains block absorbent charcoal in an inert atmosphere, naturally cools to room temperature, and inert gas selects nitrogen
Gas；
Step H: the block absorbent charcoal after hot briquetting is screened to 40-80 mesh in grinding, obtains granular mesoporous
Heat-resistant activity charcoal；
Further, the carbon source quality in the step B accounts for the percentage 30%-70% of gross mass, and template quality Zhan is total
The percentage 70%-30% of quality；
Further, the heating rate in the step C is 3-15 DEG C/min, and final temperature is 800-950 DEG C, and soaking time is
0.5-2h。
Further, the powdered mesoporous heat-resistant activity charcoal in the F-step accounts for the percentage 20%-30% of gross mass,
The quality of lithium metasilicate magnesium accounts for the percentage 5%-15% of gross mass, and distilled water accounts for the percentage 60-70% of gross mass.
Further, which is characterized in that the heating rate in the step G is 3-15 DEG C/min, final temperature 400-430
DEG C, soaking time 20-60min.
Wherein, during heating prepares powdered activated carbon, heating rate preferentially selects 5 DEG C/min, and final temperature rate is excellent
850 DEG C are first selected, soaking time preferentially selects 1h；Such heating rate is moderate, coal tar pitch can be allowed sufficiently to melt, after thawing
Coal tar pitch can wrap template magnesia, make the template action of magnesia more abundant, it is good to be conducive to preparation shape of portalling
Porous charcoal；Final temperature is 850 DEG C, is kept the temperature as 1h, under the conditions of such temperature and time, the low substance of coal tar pitch mid-boiling point holds very much
It is volatile to come out, active carbon is left, is conducive to the heat resistance and hardness that improve active carbon in this way, active carbon can be allowed to withstand
400 DEG C of thermal desorption temperatures, the existing active carbon used compared to 200-350 DEG C of thermal desorption temperature under normal circumstances, heat resistance
It can be more preferable.During powdered activated carbon is molding, forming temperature preferentially selects 400-420 DEG C, and uses crosslinking resistant to high temperature
Agent lithium metasilicate magnesium can be subjected to 500-600 DEG C of temperature, therefore granular active carbon after molding is more resistant to 400 DEG C
Temperature.
During preparing powdered activated carbon, carbon source preferentially selects coal tar pitch, and quality accounts for the percentage 30%- of gross mass
70%, template preferentially selects 80nm magnesia, and quality accounts for the percentage 70%-30% of gross mass.Such raw material ratio, Neng Gourang
Template is evenly mixed among carbon source coal tar pitch, and hot briquetting is gone after template, just will form the porous charcoal of shape of template.By
Porous charcoal after molding granulation is central hole structure, therefore crosslinking agent does not have an impact the architectural characteristic of porous charcoal, without plugging hole
Gap part, influences very little in other words.Porous charcoal aperture after molding granulation is mainly distributed on 25-100nm.Therefore active carbon symbol
Close the requirement of adsorption tube filler aperture 10-100nm.
In the preparation process of the mesoporous heat-resistant activity charcoal, need using coal tar pitch, template, hydrochloric acid etc., coal tar pitch is coking
The by-product of process is, it can be achieved that secondary use, cheap；Template magnesia is cheap；Hydrochloric acid etc. is general chemical products,
Total preparation cost is more cheap for the price of Tenax filler, is conducive to generality and popularity is promoted and used,
It can make the update alternative materials of Tenax.
Beneficial effect
1. the entire link process of preparation process realize it is controllable and adjustable so that the aperture of the active carbon is mainly divided
Cloth is central hole structure in 25-100nm, and specific surface area size is moderate；It, can be to volatile organic after being filled into adsorption tube
Gas is effectively adsorbed；Under heating and blowing state, the volatile organic compounds being adsorbed are easy desorption, realize absorption-
The continuous repetitive process of desorption can be recycled for multiple times convenient for the analysis of gas-chromatography, meet adsorption tube active carbon filler
Aperture requires.
Eventually it is 850 DEG C 2. the porous charcoal is in the preparation, keeps the temperature as 1h, such temperature and time can makes to boil in carbon source
The low substance of point volatilizees away, so that the Carbon Materials are resistant to higher temperature；During powdered activated carbon is molding, preferably
Using crosslinking agent lithium metasilicate magnesium resistant to high temperature, heat resisting temperature can reach 500-600 DEG C, further improve the temperature of the active carbon
Spend tolerance；Adsorption tube is in the link of thermal desorption, and maximum operation (service) temperature is no more than 400 DEG C；Therefore the temperature tolerance of the porous charcoal
Property enough adsorption tubes use.
3. the preparation cost of the effective mesoporous heat-resistant activity charcoal of the absorption is low, coal tar pitch is the by-product of coal process of coking,
The price of nano magnesia is not also high, and the expense of other secondary reagents is less；Therefore, the total preparation cost of the active carbon is lower,
It is expensive that business adsorbs effective Tenax filler, and there are many mesoporous heat-resistant activity charcoal cost of manufacture relative moderate, greatly
Use cost is reduced, general applicability is stronger.
Detailed description of the invention
Fig. 1 is preparation flow figure of the invention；
Fig. 2 is the nitrogen adsorption desorption curve of the hollow heat-resistant activity charcoal of powdery of the present invention；
Fig. 3 is the pore size distribution curve of powdery mesoporous heat-resistant activity charcoal of the present invention；
Fig. 4 is the nitrogen adsorption desorption curve of the hollow heat-resistant activity charcoal of graininess of the present invention；
Fig. 5 is the pore size distribution curve of graininess mesoporous heat-resistant activity charcoal of the present invention.
Specific embodiment
The present invention preferably embodiment is described in further detail below.
The powdered active carbon of several ratios is first prepared, it is de- then to carry out nitrogen suction to the powdered active carbon of different proportion
Attached experiment measures their pore property, and according to resulting pore property is tested, selection meets adsorption tube filler requirement
Active carbon is granulated, and granular mesoporous heat-resistant activity charcoal is prepared, and next uses embodiment 1, embodiment 2 and embodiment 3
It is further discussed below the preparation process of powdered activated carbon, the flow chart of preparation is as shown in Figure 1.
Embodiment 1
A kind of preparation method of mesoporous heat-resistant activity charcoal carries out in accordance with the following steps:
Blocky coal tar pitch is worn into the coal tar pitch powder of 100 mesh of partial size < by step A.；
Step B. weighs the coal tar pitch powder of 70g and the 80nm magnesia of 30g, is uniformly mixed and obtains mixing sample；
Step C. will mix sample and be fitted into corundum boat, and corundum boat is put into tube furnace；
Step D. heats above-mentioned sample in nitrogen atmosphere, and temperature program is arranged: heating rate is 5 DEG C/min, and final temperature is
850 DEG C, soaking time 1h；
Step E. clays into power the Carbon Materials fired, and powder is put into glass beaker, and the hydrochloric acid of 2mol/L is added
Soaking and stirring, the mole of hydrochloric acid are 1.2 times of template, and the soaking and stirring time is for 24 hours；It is filtered with vacuum pump and obtains powdery raw material of wood-charcoal
Material, then the Carbon Materials of powdery are placed again into clean beaker, it is subsequently added into 80 DEG C of distilled water, distilled water volume is glass
10min is stirred in the 2/3 of beaker volume, is then filtered with vacuum pump and obtains washing Carbon Materials.Water-washing step is repeated twice again,
Sufficiently remove demineralizing acid and template.
Step F. dries the Carbon Materials after pickling, and drying temperature is 105 DEG C, obtains powdery mesoporous heat-resistant activity charcoal.
Embodiment 2
The coal tar pitch powder of 50g and the 80nm magnesia of 50g are weighed, remaining step and embodiment 1 are identical.
Embodiment 3
The coal tar pitch powder of 30g and the 80nm magnesia of 70g are weighed, remaining step and embodiment 1 are identical.
Powdery mesoporous heat-resistant activity charcoal prepared by three above embodiment is subjected to the experiment of nitrogen adsorption desorption, measures them
Pore Characteristics, mainly have average pore size, specific surface area, micropore specific area and Kong Rongsi parameter.By the data of test
It is aggregated, available 1 data of table.
The experiment can also reflect: the active carbon is mesopore activated carbon, because adsorption desorption curve has apparent hysteresis loop, this
It is the typical feature of mesoporous carbon adsorption desorption curve, sees Fig. 2.The active carbon is mesopore activated carbon, and aperture is mainly distributed on 25-
100nm is shown in Fig. 3 graph of pore diameter distribution.
Table 1
| Samples | D(nm) | Sbet(m2/g) | Smic(m2/g) | Vt(cm3/g) |
| FZT73 | 5 | 19 | 9 | 0.024 |
| FZT55 | 30 | 32 | 12 | 0.239 |
| FZT37 | 23 | 86 | 35 | 0.498 |
Wherein: FZT73 is indicated are as follows: pitch powder end 70g, 80nm magnesia 30g, other ratios are similarly；D is average hole
Diameter, SbetFor the specific surface area of Carbon Materials, SmicFor the micropore specific area of Carbon Materials, VtFor the Kong Rong of Carbon Materials.
For adsorbing the active carbon of tube packing, it is desirable that: aperture is in 10-100nm, and specific surface area is in 70-200m2/ g, it is micro-
Hole proportion < 50%, Kong Rong > 0.250cm3/g。
As shown in Table 1: the average pore size < 10nm of FZT73, the average pore size for adsorbing effective active carbon is 10-100nm, because
This FZT73 is undesirable.FZT55 average pore size is that 30nm meets the requirements in the range of 10nm-100nm；Specific surface area
For 32m2/ g, not in 70-200m2In the range of/g, thus it is undesirable.FZT37 average pore size is 23nm, in 10-100nm
In range；Specific surface area is 86m2/ g, in 70-200m2In/g range；Celled portion is 35m2The total hole /g, celled portion <
50%；Kong Rongwei 0.498cm3/ g is greater than minimum requirements 0.250cm3/ g, therefore FZT37 meets the whole of adsorption tube and requires.
In conclusion the pore property of FZT37 meets absorption tube packing requirement.
Embodiment 4
Next the powdered activated carbon FZT37 for meeting absorption tube packing requirement in embodiment 1,2 and 3 is granulated.
A kind of prilling process of mesoporous heat-resistant activity charcoal carries out in accordance with the following steps:
1. weighing active carbon FZT37 prepared by 90g embodiment 3,10g lithium metasilicate magnesium is weighed, FZT37 and lithium metasilicate magnesium is equal
Even mixing adds the distilled water stirring of 300g, obtains paste samples；
2. above-mentioned paste samples are put into corundum boat, shakeout with spoon, with a thickness of 3cm, then is placed into tube furnace, to
Nitrogen is passed through in tube furnace, it is ensured that sample is in nitrogen atmosphere；
3. heating schedule is arranged, heating rate is 5 DEG C/min, and final temperature is 420 DEG C, soaking time 30min, then natural
Cooling；
4. the blocky Carbon Materials side edging of acquisition is screened to partial size 40-80 mesh, the heat-resisting mesopore activated carbon of graininess is obtained.
Embodiment 5
The optimal active carbon FZT37 of effect prepared by 80g embodiment 3 is weighed, then weighs 20g lithium metasilicate magnesium, remaining step
It is identical with embodiment 4.
Embodiment 6
The optimal active carbon FZT37 of effect prepared by 70g embodiment 3 is weighed, then weighs 30g lithium metasilicate magnesium, remaining step
It is identical with embodiment 4.
The granular activated carbon of the preparation of embodiment 4,5 and 6 is subjected to the experiment of nitrogen adsorption desorption, average pore size can be obtained, compare table
Area, micropore specific area and Kong Rong；Granular activated carbon is subjected to thermogravimetric analysis, their heat loss temperature can be obtained；It will be active
During charcoal grinds sieving, it can be seen that their frangible degree.Above-mentioned data summarization can be obtained into table 2.
The experiment can also reflect: the granular activated carbon after being granulated remains as central hole structure, because of adsorption desorption curve
Equally there is hysteresis loop, see Fig. 4.Granular activated carbon aperture after granulation is equally distributed in 25-100nm, sees Fig. 5 pore-size distribution
Figure.
Table 2
Wherein: KLT91 is indicated are as follows: FZT37 90g, lithium metasilicate magnesium 10g, other ratios are similarly；D is aperture, SbetFor charcoal
The specific surface area of material, SmicFor the micropore specific area of Carbon Materials, VtFor the Kong Rong of Carbon Materials.
For adsorbing the active carbon of tube packing, it is desirable that aperture is in 10-100nm, and specific surface area is in 70-200m2/ g, micropore
Proportion < 50%, Kong Rong > 0.250cm3/ g, heat loss temperature are greater than 400 DEG C, and active carbon quality is harder or non-friable.
As shown in Table 2: the equal > 10nm of the average pore size of three kinds of particle charcoals, adsorbing effective active carbon filler requirement is 10-
100nm, therefore meet the requirement of average pore size；The specific surface area of three kinds of granular activated carbons is in 70-200m2In/g range, because
This meets specific surface area requirement；The 50% of the micropore specific area accounting surface area of three kinds of granular activated carbons is hereinafter, meet micro-
Pore specific surface area requirement；The Kong Rongjun > 0.250cm of three kinds of granular activated carbons3/ g meets hole Rong Yaoqiu；Heat loss temperature exists
400 DEG C or more, meet heat loss temperature requirement；For intensity other than KLT91, KLT82 and KLT73's is non-friable, meets frangible
Degree requirement.
It is comprehensively compared, KLT82 and KLT73 result is ideal, meets the requirements for adsorbing effective active carbon.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is confined to these examples.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, the adjustment of several ratios can also be made, all shall be regarded as belonging to protection of the invention
Range.
Claims (5)
1. a kind of preparation method of mesoporous heat-resistant activity charcoal, it is characterised in that: including the following steps:
Step A: selecting at least one of selected from coal tar pitch and petroleum asphalt, coal tar or carbolineum to be used as carbon source, select 80nm magnesia,
At least one of 50nm magnesia or light magnesium oxide are used as template；
Step B: it with the mode of grinding by blocky coal tar pitch grinds shape, is dripped with the powdery coal that sieve filters out 100 mesh of granularity <
Blueness, adds 80nm magnesia, obtains mixing sample after mixing evenly, and mixing sample is put into corundum boat；
Step C: the corundum boat equipped with mixing sample is put into tube furnace, and heating mixing sample obtains bulk in inert gas
Carbon material then cools to room temperature, and inert gas is nitrogen, nitrogen flow 30-40ml/min；
Step D: the blocky carbon material fired of heating is pulverized shape carbon material, powdery carbon material is put into glass beaker
In, hydrochloric acid is added according to 1.1-1.3 times of 80nm magnesia mole, selecting concentration is the hydrochloric acid of 1.5-2.5mol/L, uses magnetic
Power blender stirs the mixed solution 22-26h of above-mentioned powdery carbon material and hydrochloric acid, the powdery carbon material after pickling is obtained by filtration,
Powdery carbon material after pickling is placed again into clean glass beaker, the distilled water that water temperature is 70-90 DEG C is added, distillation
The volume of water is the 2/3-4/5 of beaker capacity, stirs 5-10min, and be filtered, and the process of distillation washing carbon repeats 2-3 times,
Powdery carbon material after obtaining template；
Step E: being dried going the powdery carbon material after template to be put into drying box, and drying temperature is 100-110 DEG C, obtains
Dry powdery mesoporous heat-resistant activity charcoal；
Step F: powdery mesoporous heat-resistant activity charcoal, crosslinking agent and distilled water are mixed according to mass percent, are evenly stirred until paste
Shape obtains pasty mixture, and crosslinking agent selects lithium metasilicate magnesium；
Step G: pasty mixture is spread in corundum boat with spoon, keeps the thickness of pasty mixture uniform, and with a thickness of 3-
4cm, then hot briquetting obtains block absorbent charcoal in an inert atmosphere, naturally cools to room temperature, and inert gas selects nitrogen；
Step H: the block absorbent charcoal after hot briquetting is screened to 40-80 mesh in grinding, it is heat-resisting to obtain granular mesoporous
Active carbon.
2. a kind of preparation method of mesoporous heat-resistant activity charcoal as described in claim 1, which is characterized in that in the step B
Carbon source quality accounts for the percentage 30%-70% of gross mass, and template quality accounts for the percentage 70%-30% of gross mass.
3. a kind of preparation method of mesoporous heat-resistant activity charcoal according to claim 1, which is characterized in that in the step C
Heating rate be 3-15 DEG C/min, 800-950 DEG C of final temperature, soaking time 0.5-2h.
4. a kind of preparation method of mesoporous heat-resistant activity charcoal according to claim 1, which is characterized in that in the F-step
Powdered mesoporous heat-resistant activity charcoal account for the percentage 20%-30% of gross mass, the quality of lithium metasilicate magnesium accounts for the percentage of gross mass
Than 5%-15%, distilled water accounts for the percentage 60-70% of gross mass.
5. a kind of preparation method of mesoporous heat-resistant activity charcoal according to claim 1, which is characterized in that in the step G
Heating rate be 3-15 DEG C/min, 400-430 DEG C of final temperature, soaking time 20-60min.
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| CN112850707A (en) * | 2021-02-05 | 2021-05-28 | 汪炜 | Preparation method of activated carbon |
| CN115184443A (en) * | 2022-06-15 | 2022-10-14 | 新疆大学 | Preparation method and application of electrochemical sensor for detecting nitrophenol in actual water body |
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