CN101445232A - Porous carbon and preparation method thereof - Google Patents
Porous carbon and preparation method thereof Download PDFInfo
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- CN101445232A CN101445232A CNA2008102270156A CN200810227015A CN101445232A CN 101445232 A CN101445232 A CN 101445232A CN A2008102270156 A CNA2008102270156 A CN A2008102270156A CN 200810227015 A CN200810227015 A CN 200810227015A CN 101445232 A CN101445232 A CN 101445232A
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Abstract
The invention discloses a porous carbon and a preparation method thereof. The preparation method of the porous carbon comprises the following steps: 1) 1 part by weight of petroleum residual oil and 3-9 parts by weight or organic magnesium salt are mixed and smashed, and then the temperature is increased to 700-1000 DEG C for carbonization for 1-2 hours, thereby obtaining carbonized products; the pressure of inert gas during the carbonization is 100kPa-105kPa; 2) the acid treatment is carried out on the carbonized products, then the carbonized products are washed until neutral, and the porous carbon is obtained after drying. The porous carbon obtained by the invention has high specific surface area (up to 1183m<2>/g) and good absorption performance; furthermore, the pore size can be regulated and controlled according to the needs of applications. The preparation method has the following advantages: the preparation method does not need to carry out the stabilization and the activation processes, and the operation is simple and easy; magnesium oxide particles generated after the carbonization are easy to remove and can be removed by weak acetic acid, thereby being capable of realizing the recycling of magnesium acetate and reducing the production cost; and the yield of the porous carbon is higher.
Description
Technical field
The present invention relates to a kind of porous charcoal and preparation method thereof.
Background technology
Porous charcoal is used very extensive in industrial production and daily life as sorbent material commonly used.At present, porous charcoal generally is with feedstock production such as coal, timber and shells, and along with the raising of people's ecotope consciousness, it is more and more that raw materials such as employing natural phant and mineral are prepared the restriction that is subjected to.
And petroleum residual oil is as the by product of petroleum industry, and it is very extensive to originate, and the annual production of whole world residual oil is about 6～700,000,000 tons, most ofly directly burnt by the oil that directly acts as a fuel.
In the porous charcoal patent that existing oil is, mostly being with refinery coke and petroleum pitch is raw material.As patent CN1030736A refinery coke is pulverized the back and heated 1～3 hour down at 500～800 ℃, cooling back crushing screening can obtain porous charcoal, and the characteristics of this patent are that complete processing is simple, operate simple and easy.Patent CN101028923A pulverizes refinery coke after pre-oxidation treatment; with the alkali metal hydroxide activation, make super-activated carbon after washing and the drying under inert atmosphere protection, the characteristics of this patent are the operation of refinery coke through preoxidation; can reduce the consumption of alkaline activation agent, save cost.Patent CN1927709A is raw material with the mid-temperature pitch, be dissolved in the methylene dichloride, its appendix is heat-treated on the flesh skeleton in stalk, with potassium hydroxide is activator, after 1～2 hour, make gac 700～900 ℃ of activation after washing drying, the characteristics of this patent are to adopt mid-temperature pitch, and shortened heat treatment time, reduced energy consumption.
Summary of the invention
The purpose of this invention is to provide a kind of porous charcoal and preparation method thereof.
The preparation method of porous charcoal provided by the invention may further comprise the steps:
1) 1 mass parts petroleum residual oil and the broken back of the organic magnesium salts powder mix of 3-9 mass parts were warming up in inert atmosphere 700-1000 ℃ of charing 1-2 hour, obtain carbonizing production; Gaseous tension is 100kPa～105kPa in the described inert atmosphere;
2) carbonizing production is carried out acid treatment, be washed till neutrality then, can obtain porous charcoal after the drying.
Described method specifically can comprise the steps:
1) 1 mass parts petroleum residual oil and the broken back of the organic magnesium salts powder mix of 3-9 mass parts are warming up to 900 ℃ of charings 1 hour in inert atmosphere, obtain carbonizing production; Gaseous tension is 103kPa in the described inert atmosphere;
2) carbonizing production is carried out acid treatment, be washed till neutrality then, can obtain porous charcoal after the drying.
Described step 2) neutrality in refers to pH6-8, preferred pH7.
Described organic magnesium salts specifically can be magnesium acetate and/or magnesium citrate.
Used acid-specific can be sulfuric acid and/or hydrochloric acid in the described acid treatment.
Used acid is preferably the sulfuric acid of 2mol/L, the hydrochloric acid of 1mol/L or the hydrochloric acid of 2mol/L in the described acid treatment.
Described rare gas element specifically can be nitrogen and/or argon gas.
In the described step 1), temperature rise rate can be 2～15 ℃/min, preferred 5 ℃/min.
In order to make the porous charcoal specific surface area higher, the processing of can sieving after described petroleum residual oil and organic magnesium salts powder mix are broken; The aperture of described sieve can be 200～300 orders, is preferably 300 orders.
Described step 2) in, can carry out drying under field conditions (factors), for pick up speed, also can adopt high temperature drying, as the high temperature drying more than 100 ℃.
The porous charcoal that described method prepares also belongs to protection scope of the present invention.
The by product of petroleum industry-petroleum residual oil carbon content height, ash oontent is low, is a kind of charcoal source of good preparation porous charcoal.Petroleum residual oil and organic magnesium salts are mixed directly charing of back, generate charcoal and magnesian mixture after the charing, can make porous charcoal behind the magnesium oxide with the generation of diluted acid flush away.The porous charcoal specific surface area height that the present invention obtains (can reach 1200m
2/ g), good adsorption performance, and the aperture can be regulated and control according to application need.Preparation method of the present invention has following advantage: need not stabilization and reactivation process, simple, easy handling; The magnesium oxide particle that generates after the charing is easy to remove, and can remove with weak acid, can realize magnesian recycle, reduces production cost; The porous charcoal yield is higher.
Following embodiment is convenient to understand better the present invention, but does not limit the present invention.
Description of drawings
Fig. 1 is the porous charcoal of embodiment 1 preparation; (a) stereoscan photograph before the flush away MgO; (b) stereoscan photograph behind the flush away MgO.
Embodiment
Experimental technique among the following embodiment if no special instructions, is ordinary method.
The method of testing product performance is as follows in following examples:
Yield (%): porous charcoal quality/residual oil quality * 100%.
Specific surface area (m
2/ g): adopt the method for nitrogen absorption, obtain by the BET equation.
Total hole volume (cm
2/ g): adopt the method for nitrogen absorption, total hole volume (V
Total) be to be p/p with relative pressure
0=0.95 o'clock nitrogen adsorption amount is converted to the liquid nitrogen volume and obtains.
Middle pore volume (cm
2/ g): adopt the method for nitrogen absorption, obtain micropore pore volume (V by t figure method
Micro), middle pore volume (V
Meso) obtain according to the difference of total pore volume and micropore pore volume.
Mean pore size (A): adopt the method for nitrogen absorption, calculate by specific surface area and total hole volume.
The preparation of embodiment 1, porous charcoal and performance measurement
Test is provided with 3 repetitions, the results averaged of Performance Detection.
One, the preparation of porous charcoal
1, the mass ratio of petroleum residual oil and magnesium acetate being pressed 1:3 mixes, and with the broken back of pneumatic abrasive dust 300 mesh sieves excessively, is warming up to 1000 ℃ in the nitrogen atmosphere (nitrogen pressure is 103kPa) then, and charing 1 hour obtains carbonizing production.Temperature rise rate is 5 ℃/min.The stereoscan photograph of carbonizing production is seen Fig. 1 (a).
2, carbonizing production is washed with the 2mol/L dilute sulphuric acid, be washed till neutrality (pH7) with deionized water then, dry under 100 ℃, obtain product A.The stereoscan photograph of product A is seen Fig. 1 (b).
Two, the performance measurement of porous charcoal
The performance of product A sees Table 1.
The performance of table 1 product A
| Yield (%) | Specific surface area (m 2/g) | Total hole volume (cm 2/g) | Middle pore volume (cm 2/g) | Mean pore size (nm) |
| 27.3 | 1183 | 1.80 | 1.75 | 6.1 |
The preparation of embodiment 2, porous charcoal and performance measurement
Test is provided with 3 repetitions, the results averaged of Performance Detection.
1, the mass ratio of petroleum residual oil and magnesium acetate being pressed 1:9 mixes, and with the broken back of pneumatic abrasive dust 200 mesh sieves excessively, is warming up to 700 ℃ in the nitrogen atmosphere (nitrogen pressure is 100kPa) then, and charing 2 hours obtains carbonizing production.Temperature rise rate is 2 ℃/min.
2, carbonizing production is washed with 1mol/L dilute hydrochloric acid, be washed till neutrality (pH6) with deionized water then, dry under 100 ℃, obtain product B.
Two, the performance measurement of porous charcoal
The performance of product B sees Table 2.
The performance of table 2 product B
| Yield (%) | Specific surface area (m 2/g) | Total hole volume (cm 2/g) | Middle pore volume (cm 2/g) | Mean pore size (nm) |
| 29.5 | 1050 | 1.75 | 1.71 | 6.6 |
The preparation of embodiment 3, porous charcoal and performance measurement
Test is provided with 3 repetitions, the results averaged of Performance Detection.
One, the preparation of porous charcoal
1, the mass ratio of petroleum residual oil and magnesium acetate being pressed 1:5 mixes, and with the broken back of pneumatic abrasive dust 250 mesh sieves excessively, is warming up to 850 ℃ in the argon gas atmosphere (argon pressure is 105kPa) then, and charing 1.5 hours obtains carbonizing production.Temperature rise rate is 15 ℃/min.
2, carbonizing production is washed with the 2mol/L dilute sulphuric acid, be washed till neutrality (pH8) with deionized water then, dry under 100 ℃, obtain products C.
Two, the performance measurement of porous charcoal
The performance of products C sees Table 3.
The performance of table 3 products C
| Yield (%) | Specific surface area (m 2/g) | Total hole volume (cm 2/g) | Middle pore volume (cm 2/g) | Mean pore size (nm) |
| 28.2 | 960 | 1.56 | 1.50 | 6.5 |
The preparation of embodiment 4, porous charcoal and performance measurement
Test is provided with 3 repetitions, the results averaged of Performance Detection.
One, the preparation of porous charcoal
1, the mass ratio of petroleum residual oil and magnesium citrate being pressed 1:9 mixes, and with the broken back of pneumatic abrasive dust 300 mesh sieves excessively, is warming up to 900 ℃ in the nitrogen atmosphere (nitrogen pressure is 103kPa) then, and charing 1 hour obtains carbonizing production.Temperature rise rate is 5 ℃/min.
2, carbonizing production is washed with 2mol/L dilute hydrochloric acid, be washed till neutrality (pH6.5) with deionized water then, dry under 100 ℃, obtain product D.
Two, the performance measurement of porous charcoal
The performance of product D sees Table 4.
The performance of table 4 product D
| Yield (%) | Specific surface area (m 2/g) | Total hole volume (cm 2/g) | Middle pore volume (cm 2/g) | Mean pore size (nm) |
| 66.7％ | 1032 | 2.70 | 2.60 | 105 |
The preparation of embodiment 5, porous charcoal and performance measurement
Test is provided with 3 repetitions, the results averaged of Performance Detection.
One, the preparation of porous charcoal
1, the mass ratio of petroleum residual oil and magnesium citrate being pressed 1:3 mixes, and with the broken back of pneumatic abrasive dust 200 mesh sieves excessively, is warming up to 800 ℃ in the nitrogen atmosphere (nitrogen pressure is 105kPa) then, and charing 1.5 hours obtains carbonizing production.Temperature rise rate is 15 ℃/min.
2, carbonizing production is washed with 2mol/L dilute hydrochloric acid, be washed till neutrality (pH7.5) with deionized water then, dry under 100 ℃, obtain product E.
Two, the performance measurement of porous charcoal
The performance of product E sees Table 5.
The performance of table 5 product E
| Yield (%) | Specific surface area (m 2/g) | Total hole volume (cm 2/g) | Micropore volume (cm 2/g) | Mean pore size (nm) |
| 59.5 | 768 | 1.95 | 1.90 | 10.2 |
Claims (10)
1, a kind of preparation method of porous charcoal may further comprise the steps:
1) 1 mass parts petroleum residual oil and the broken back of the organic magnesium salts powder mix of 3-9 mass parts were warming up in inert atmosphere 700-1000 ℃ of charing 1-2 hour, obtain carbonizing production; Gaseous tension is 100kPa～105kPa in the described inert atmosphere;
2) carbonizing production is carried out acid treatment, be washed till neutrality then, can obtain porous charcoal after the drying.
2, the method for claim 1 is characterized in that: described method comprises the steps:
1) 1 mass parts petroleum residual oil and the broken back of the organic magnesium salts powder mix of 3-9 mass parts are warming up to 900 ℃ of charings 1 hour in inert atmosphere, obtain carbonizing production; Gaseous tension is 103kPa in the described inert atmosphere;
2) carbonizing production is carried out acid treatment, be washed till neutrality then, can obtain porous charcoal after the drying.
3, method as claimed in claim 1 or 2 is characterized in that: described organic magnesium salts is magnesium acetate and/or magnesium citrate.
4, as arbitrary described method in the claim 1 to 3, it is characterized in that: used acid is sulfuric acid and/or hydrochloric acid in the described acid treatment.
5, method as claimed in claim 4 is characterized in that: used acid is the sulfuric acid of 2mol/L, the hydrochloric acid of 1mol/L or the hydrochloric acid of 2mol/L in the described acid treatment.
6, as arbitrary described method in the claim 1 to 5, it is characterized in that: described rare gas element is nitrogen and/or argon gas.
7, as arbitrary described method in the claim 1 to 6, it is characterized in that: in the described step 1), temperature rise rate is 2～15 ℃/min.
8, method as claimed in claim 7 is characterized in that: in the described step 1), temperature rise rate is 5 ℃/min.
9, as arbitrary described method in the claim 1 to 8, it is characterized in that: sieve after described petroleum residual oil and organic magnesium salts powder mix are broken; The aperture of described sieve is 200～300 orders, preferred 300 orders.
10, the porous charcoal that arbitrary described method prepares in the claim 1 to 9.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106170457A (en) * | 2014-03-12 | 2016-11-30 | 东洋炭素株式会社 | Porous carbon, its manufacture method and the adsorption/desorption device of use porous carbon |
| CN106495127A (en) * | 2016-11-15 | 2017-03-15 | 河南理工大学 | A kind of simple method for preparing of mesoporous carbon |
| CN106914267A (en) * | 2017-03-31 | 2017-07-04 | 温州大学 | A kind of nitrogen co-doped mesoporous carbon of iron and its preparation method and application |
| CN107176655A (en) * | 2017-04-11 | 2017-09-19 | 北京化工大学 | A kind of method of utilization block foam structure chelate synthesis multi-stage porous carbon electric adsorption electrode material and application |
| CN107720724A (en) * | 2017-11-16 | 2018-02-23 | 西安交通大学 | A kind of high surface area nano-porous carbon material and preparation method thereof |
| CN110028050A (en) * | 2019-04-17 | 2019-07-19 | 东南大学 | A method of supercapacitor Carbon Materials are prepared using bio oil |
| CN111530440A (en) * | 2020-05-07 | 2020-08-14 | 中国矿业大学 | Preparation method of coal-based porous material |
| CN112645307A (en) * | 2021-01-28 | 2021-04-13 | 太原理工大学 | Method for preparing hydrophilic carbon material |
| CN112713271A (en) * | 2020-12-29 | 2021-04-27 | 上海杉杉科技有限公司 | Modified graphite material, preparation method thereof, lithium ion battery and application |
-
2008
- 2008-11-18 CN CNA2008102270156A patent/CN101445232A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106170457A (en) * | 2014-03-12 | 2016-11-30 | 东洋炭素株式会社 | Porous carbon, its manufacture method and the adsorption/desorption device of use porous carbon |
| CN106495127A (en) * | 2016-11-15 | 2017-03-15 | 河南理工大学 | A kind of simple method for preparing of mesoporous carbon |
| CN106914267A (en) * | 2017-03-31 | 2017-07-04 | 温州大学 | A kind of nitrogen co-doped mesoporous carbon of iron and its preparation method and application |
| CN107176655A (en) * | 2017-04-11 | 2017-09-19 | 北京化工大学 | A kind of method of utilization block foam structure chelate synthesis multi-stage porous carbon electric adsorption electrode material and application |
| CN107176655B (en) * | 2017-04-11 | 2020-05-19 | 北京化工大学 | Method for synthesizing hierarchical porous carbon electro-adsorption electrode material by using block-shaped foam structure chelate and application |
| CN107720724A (en) * | 2017-11-16 | 2018-02-23 | 西安交通大学 | A kind of high surface area nano-porous carbon material and preparation method thereof |
| CN107720724B (en) * | 2017-11-16 | 2019-12-24 | 西安交通大学 | Nano porous carbon material with high specific surface area and preparation method thereof |
| CN110028050A (en) * | 2019-04-17 | 2019-07-19 | 东南大学 | A method of supercapacitor Carbon Materials are prepared using bio oil |
| CN111530440A (en) * | 2020-05-07 | 2020-08-14 | 中国矿业大学 | Preparation method of coal-based porous material |
| CN112713271A (en) * | 2020-12-29 | 2021-04-27 | 上海杉杉科技有限公司 | Modified graphite material, preparation method thereof, lithium ion battery and application |
| CN112645307A (en) * | 2021-01-28 | 2021-04-13 | 太原理工大学 | Method for preparing hydrophilic carbon material |
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