CN105197927A - Preparation method of mesoporous activated carbon - Google Patents
Preparation method of mesoporous activated carbon Download PDFInfo
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- CN105197927A CN105197927A CN201510639156.9A CN201510639156A CN105197927A CN 105197927 A CN105197927 A CN 105197927A CN 201510639156 A CN201510639156 A CN 201510639156A CN 105197927 A CN105197927 A CN 105197927A
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Abstract
The invention discloses a preparation method of mesoporous activated carbon. The preparation method includes: soaking sawdust in treating liquid, rising temperature to 50-60 DEG C, and stirring for 10-20 minutes; rising temperature to 100-120 DEG C under a vacuum condition, allowing standing for 40-50 minutes, and lowering temperature to room temperature; adding diethyltoluenediamine, and mixing well to obtain a first material; rising temperature of the first material to 600-650 DEG C under a condition of nitrogen protection, and maintaining for 150-200 minutes; lowering temperature to room temperature to obtain a carbonized material; soaking the carbonized material in a diethylamine water solution, rising temperature to 30-40 DEG C, and maintaining the temperature for 100-120 minutes; filtering, using deionized water to wash until pH does not change, and drying to obtain the mesoporous activated carbon. The mesoporous activated carbon obtained by the preparation method has good performance, and applicability is improved.
Description
Technical field
The invention belongs to gac preparing technical field, be specifically related to a kind of preparation method of mesoporous activated carbon.
Background technology
Gac is also known as active black.Be black powder or bulk, particulate state, cellular decolorizing carbon, also have the crystal carbon that arrangement is regular.In gac except carbon, also comprise two class admixtures: a class is chemically combined element, mainly oxygen and hydrogen, these elements remain in charcoal owing to not carbonizing completely, or in reactivation process, external non-carbon is combined with Surface Chemistry of Activated Carbon, during as used steam activation, and the oxidized or steam oxidation of activated carbon surface; Another kind of admixture is ash content, and it is the inorganic part of gac; Ash content easily causes secondary pollution in activated carbon.The main raw material of gac can be almost all organic materialss being rich in carbon, as coal, timber, shell, coconut husk, nut-shell, apricot shell, jujube shell etc.These carbonaceous materials, in activation furnace, are converted into gac by pyrolysis under high temperature and certain pressure.
Gac is because having high-specific surface area, micropore-advantage such as macroporous structure and low density and receiving publicity.The technical field such as be at present widely used in support of the catalyst, energy storage, absorption and be separated.Biomass comprise the raw material that Exocarpium cocois (Cocos nucifera L), bamboo bits and timber all can be used as producing gac.The surface topography of gac and Pore structure and morphology determine its application at emerging field.Therefore, the special construction of design and structure gac seems particularly important.As the alternative techniques of high temperature pyrolysis (~ 800 DEG C), hydro-thermal charing (>200 DEG C) technique is for the preparation of functionalization absorbent charcoal material (Sevillaetal.Carbon, 2009 with specific structural features; 47 (9): 2281).Had now a series of gac through hydro-thermal charing preparation, take carbohydrate as raw material usually, preparation temperature is 170 ~ 240 DEG C, obtains highly homogeneous spherical carbon particle (0.4 ~ 0.6 μm).But this technique still exists some shortcomings, as needed high-tension apparatus, product structure single.Wood materials is utilized to prepare the method for gac at present existing a lot, but the method for the good mesoporous activated carbon of processability few, and the gac simultaneously prepared does not reach good specific surface area, thus have impact on adsorption effect yet.
Summary of the invention
The object of the invention is to the preparation method that a kind of mesoporous activated carbon is provided to overcome above the deficiencies in the prior art, promoting the properties of the product prepared.
Technical scheme of the present invention is as follows:
A preparation method for mesoporous activated carbon, comprises the following steps:
Step one, wood chip is dipped in treatment solution, be warming up to 50-60 DEG C, stir 10-20 minute, be then warming up to 100-120 DEG C under vacuum, leave standstill 40-50 minute, be down to room temperature, then add diethyl toluene diamine, mix, obtain material one, wherein treatment solution is the mixture of 4-chloro-butyric acid, Tetra hydro Phthalic anhydride and water;
Step 2, is warming up to 600-650 DEG C by material one under the condition of nitrogen protection, keeps 150-200 minute, is then down to room temperature, obtains carbonized material;
Step 3, is immersed in carbonized material in ethylenediamine solution, is warming up to 30-40 DEG C, and constant temperature keeps 100-120 minute, then filters, does not change with deionized water wash to pH, dries, obtains mesoporous activated carbon.
The preparation method of described mesoporous activated carbon, in step one, the vacuum tightness of vacuum condition is 0.003-0.01MPa.
The preparation method of described mesoporous activated carbon, the mass ratio of the quality and wood chip that add diethyl toluene diamine in step one is 0.1-0.3:2.
The preparation method of described mesoporous activated carbon, in step one treatment solution, the mass ratio of 4-chloro-butyric acid, Tetra hydro Phthalic anhydride and water is 2-5:1-3:6-10.
The preparation method of described mesoporous activated carbon, the heat-up rate being warming up to 600-650 DEG C in step 2 is 15-20 DEG C/min.
The preparation method of described mesoporous activated carbon, in step 3, the mass concentration of ethylenediamine solution is 8-12%.
The preparation method of described mesoporous activated carbon, is characterized in that, in step 3, bake out temperature is 100-120 DEG C.
The mesoporous activated carbon that preparation method provided by the invention obtains has good performance, and its mesoporous reaches about 4nm, and specific surface area reaches 2280m
2/ more than g, ash content reaches less than 3.25%.
Embodiment:
Embodiment 1
A preparation method for mesoporous activated carbon, comprises the following steps:
Step one, 400g wood chip is dipped in treatment solution, being warming up to 50 DEG C, stirring 10 minutes, is then be warming up to 100 DEG C under the vacuum condition of 0.003MPa in vacuum tightness, leave standstill 40 minutes, be down to room temperature, then add diethyl toluene diamine 20g, mix, obtain material one, wherein treatment solution is the mixture of 600g4-chloro-butyric acid, 300g Tetra hydro Phthalic anhydride and 1800g water;
Step 2, is warming up to 600 DEG C by material one under the condition of nitrogen protection, and heat-up rate is 15 DEG C/min, keeps 150 minutes, is then down to room temperature, obtains carbonized material;
Step 3, carbonized material being immersed in mass concentration is in the ethylenediamine solution of 8%, and be warming up to 30 DEG C, constant temperature keeps 100 minutes, then filters, and does not change to pH with deionized water wash, and dry, bake out temperature is 100 DEG C, obtains mesoporous activated carbon.
Embodiment 2
A preparation method for mesoporous activated carbon, comprises the following steps:
Step one, 400g wood chip is dipped in treatment solution, being warming up to 53 DEG C, stirring 15 minutes, is then be warming up to 108 DEG C under the vacuum condition of 0.004MPa in vacuum tightness, leave standstill 44 minutes, be down to room temperature, then add 30g diethyl toluene diamine, mix, obtain material one, wherein treatment solution is the mixture of 500g4-chloro-butyric acid, 300g Tetra hydro Phthalic anhydride and 1600g water;
Step 2, is warming up to 620 DEG C by material one under the condition of nitrogen protection, and heat-up rate is 16 DEG C/min, keeps 160 minutes, is then down to room temperature, obtains carbonized material;
Step 3, carbonized material being immersed in mass concentration is in the ethylenediamine solution of 9%, and be warming up to 33 DEG C, constant temperature keeps 106 minutes, then filters, and does not change to pH with deionized water wash, and dry, bake out temperature is 105 DEG C, obtains mesoporous activated carbon.
Embodiment 3
A preparation method for mesoporous activated carbon, comprises the following steps:
Step one, 400g wood chip is dipped in treatment solution, being warming up to 58 DEG C, stirring 16 minutes, is then be warming up to 112 DEG C under the vacuum condition of 0.006MPa in vacuum tightness, leave standstill 46 minutes, be down to room temperature, then add 50g diethyl toluene diamine, mix, obtain material one, wherein treatment solution is the mixture of 600g4-chloro-butyric acid, 350g Tetra hydro Phthalic anhydride and 1600g water;
Step 2, is warming up to 640 DEG C by material one under the condition of nitrogen protection, and heat-up rate is 20 DEG C/min, keeps 180 minutes, is then down to room temperature, obtains carbonized material;
Step 3, carbonized material being immersed in mass concentration is in the ethylenediamine solution of 10%, and be warming up to 38 DEG C, constant temperature keeps 115 minutes, then filters, and does not change to pH with deionized water wash, and dry, bake out temperature is 110 DEG C, obtains mesoporous activated carbon.
Embodiment 4
A preparation method for mesoporous activated carbon, comprises the following steps:
Step one, 600g wood chip is dipped in treatment solution, being warming up to 60 DEG C, stirring 20 minutes, is then be warming up to 120 DEG C under the vacuum condition of 0.01MPa in vacuum tightness, leave standstill 50 minutes, be down to room temperature, then add 90g diethyl toluene diamine, mix, obtain material one, wherein treatment solution is the mixture of 1000g4-chloro-butyric acid, 600g Tetra hydro Phthalic anhydride and 2000g water;
Step 2, is warming up to 650 DEG C by material one under the condition of nitrogen protection, and heat-up rate is 20 DEG C/min, keeps 200 minutes, is then down to room temperature, obtains carbonized material;
Step 3, carbonized material being immersed in mass concentration is in the ethylenediamine solution of 12%, and be warming up to 40 DEG C, constant temperature keeps 120 minutes, then filters, and does not change to pH with deionized water wash, and dry, bake out temperature is 100-120 DEG C, obtains mesoporous activated carbon.
The mesoporous activated carbon prepared for above embodiment carries out performance test, and result is as following table:
| Project | Aperture/nm | Specific surface area/m 2/g | Ash content/% |
| Embodiment 1 | 4.2 | 2280 | 3.25 |
| Embodiment 2 | 3.8 | 2310 | 3.18 |
| Embodiment 3 | 3.5 | 2360 | 3.06 |
| Embodiment 4 | 3.7 | 2345 | 3.10 |
As can be seen from the above results, the mesoporous activated carbon that preparation method provided by the invention obtains has good performance, and its mesoporous reaches about 4nm, and specific surface area reaches 2280m
2/ more than g, ash content reaches less than 3.25%, and researchist finds in the process of the present invention's exploitation, and the present invention is by processing prepared using treatment solution, improve homogeneity and the specific surface area of the pore-forming finally obtaining absorbent charcoal material, preparation process is more easily controlled.
In sum, the gac that preparation method provided by the invention obtains has good performance, improves application efficiency.
Claims (7)
1. a preparation method for mesoporous activated carbon, is characterized in that, comprises the following steps:
Step one, wood chip is dipped in treatment solution, be warming up to 50-60 DEG C, stir 10-20 minute, be then warming up to 100-120 DEG C under vacuum, leave standstill 40-50 minute, be down to room temperature, then add diethyl toluene diamine, mix, obtain material one, wherein treatment solution is the mixture of 4-chloro-butyric acid, Tetra hydro Phthalic anhydride and water;
Step 2, is warming up to 600-650 DEG C by material one under the condition of nitrogen protection, keeps 150-200 minute, is then down to room temperature, obtains carbonized material;
Step 3, is immersed in carbonized material in ethylenediamine solution, is warming up to 30-40 DEG C, and constant temperature keeps 100-120 minute, then filters, does not change with deionized water wash to pH, dries, obtains mesoporous activated carbon.
2. the preparation method of mesoporous activated carbon according to claim 1, is characterized in that, in step one, the vacuum tightness of vacuum condition is 0.003-0.01MPa.
3. the preparation method of mesoporous activated carbon according to claim 1, is characterized in that, the mass ratio of the quality and wood chip that add diethyl toluene diamine in step one is 0.1-0.3:2.
4. the preparation method of mesoporous activated carbon according to claim 1, is characterized in that, in step one treatment solution, the mass ratio of 4-chloro-butyric acid, Tetra hydro Phthalic anhydride and water is 2-5:1-3:6-10.
5. the preparation method of mesoporous activated carbon according to claim 1, is characterized in that, the heat-up rate being warming up to 600-650 DEG C in step 2 is 15-20 DEG C/min.
6. the preparation method of mesoporous activated carbon according to claim 1, is characterized in that, in step 3, the mass concentration of ethylenediamine solution is 8-12%.
7. the preparation method of mesoporous activated carbon according to claim 1, is characterized in that, in step 3, bake out temperature is 100-120 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106608626A (en) * | 2016-12-16 | 2017-05-03 | 陕西中医药大学 | Method for preparing jujube pit active carbon through phosphoric acid activation |
| CN106986337A (en) * | 2016-12-23 | 2017-07-28 | 镇江华域环保设备制造有限公司 | A kind of preparation method of air cleaning porous activated carbon |
| CN109081341A (en) * | 2018-09-30 | 2018-12-25 | 江苏斯沃得环保科技有限公司 | A kind of preparation method of mesoporous activated carbon |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648707A (en) * | 2009-08-27 | 2010-02-17 | 南京林业大学 | Preparation method of activated carbon with high pore volume |
| CN103359729A (en) * | 2013-08-01 | 2013-10-23 | 中国科学院西双版纳热带植物园 | Novel preparation method of mesoporous active carbon |
| CN103408007A (en) * | 2013-07-26 | 2013-11-27 | 福建农林大学 | Method for preparing nitrogen-doped activated carbon by using melamine waste |
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- 2015-09-30 CN CN201510639156.9A patent/CN105197927B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648707A (en) * | 2009-08-27 | 2010-02-17 | 南京林业大学 | Preparation method of activated carbon with high pore volume |
| CN103408007A (en) * | 2013-07-26 | 2013-11-27 | 福建农林大学 | Method for preparing nitrogen-doped activated carbon by using melamine waste |
| CN103359729A (en) * | 2013-08-01 | 2013-10-23 | 中国科学院西双版纳热带植物园 | Novel preparation method of mesoporous active carbon |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106608626A (en) * | 2016-12-16 | 2017-05-03 | 陕西中医药大学 | Method for preparing jujube pit active carbon through phosphoric acid activation |
| CN106986337A (en) * | 2016-12-23 | 2017-07-28 | 镇江华域环保设备制造有限公司 | A kind of preparation method of air cleaning porous activated carbon |
| CN109081341A (en) * | 2018-09-30 | 2018-12-25 | 江苏斯沃得环保科技有限公司 | A kind of preparation method of mesoporous activated carbon |
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Effective date of registration: 20210105 Address after: 212434 no.1169, airport new area, Guozhuang Town, Jurong City, Zhenjiang City, Jiangsu Province Patentee after: Jiangsu fuhuitong Environmental Protection Technology Co.,Ltd. Address before: No. 688, Dongfanghong village, Guozhuang Town, Jurong City, Zhenjiang City, Jiangsu Province, 212434 Patentee before: JIANGSU TONGRUI ENVIRONMENTAL PROTECTION TECHNOLOGY DEVELOPMENT Co.,Ltd. |
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