CN105197929A - Method for preparing activated carbon with large specific surface area from sawdust - Google Patents
Method for preparing activated carbon with large specific surface area from sawdust Download PDFInfo
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- CN105197929A CN105197929A CN201510642974.4A CN201510642974A CN105197929A CN 105197929 A CN105197929 A CN 105197929A CN 201510642974 A CN201510642974 A CN 201510642974A CN 105197929 A CN105197929 A CN 105197929A
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- surface area
- specific surface
- materials
- wood chip
- hydrochloric acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/78—Recycling of wood or furniture waste
Abstract
The invention discloses a method for preparing activated carbon with a large specific surface area from sawdust. The method includes arranging the sawdust in a reflux device, adding mixed liquid of ethyl acetate and absolute ethyl alcohol into the reflux device, carrying out heating reflux for 120-150 minutes and filtering the sawdust and the mixed liquid to obtain solid mixtures; carbonizing the solid mixtures in a carbonizing furnace to obtain carbonized materials; immersing the carbonized materials in hydrochloric acid solution, keeping the carbonized materials in the hydrochloric acid solution for 50-80 minutes, filtering the carbonized materials and the hydrochloric acid solution to obtain solid substances and cleaning the filtered solid substances by the aid of deionized water to obtain first materials; enabling the first materials, triethylamine and 2-methyl-1, 3-butadiene to react with one another to obtain reaction products, filtering the reaction products to obtain solid substances, immersing the filtered solid substances in hydrochloric acid solution, keeping the solid substances in the hydrochloric acid solution for certain time and then filtering the solid substances to obtain second materials; cleaning the second materials by the aid of deionized water, heating the second materials under the condition of nitrogen protection, keeping heating the second materials for certain time and cooling the second materials until the temperatures of the second materials reach the room temperature so as to obtain the activated carbon. The method has the advantages that the activated carbon with the large specific surface area can be prepared by the aid of the method, and accordingly application requirements can be effectively met.
Description
Technical field
The invention belongs to gac preparing technical field, be specifically related to a kind of method utilizing wood chip to prepare active carbon with high specific surface area.
Background technology
Gac is with fat coal, wood chip or shell for raw material, through a kind of porousness charcoal element material that the technological processs such as machine-shaping, charing, activation are made.It has certain physical strength, very large specific surface area and extremely strong absorption property.Energy decolouring, deodorization, desulfurization, de-benzene, optionally can also remove some impurity atom and mechanical impurity in liquid phase or gas phase.Also can adsorb some catalyzer, chemical reaction velocity is accelerated greatly, be good support of the catalyst.Therefore gac has purposes widely in all respects of national defence, chemical industry, oil, weaving, food, medicine, nuclear industry, urban construction, environment protection and human lives.Granular carbon performance and purposes.Active carbon with high specific surface area is in the large-scale production eighties in last century, and its performance is significantly better than conventional gac, but the general specific surface area of active carbon with high specific surface area conventional is at present at 3000m
2within/g, along with the development of industry, in some occasion as its performance of the storage request of hydrogen especially specific surface area still needs further lifting.
Summary of the invention
The object of the invention is to provide a kind of method utilizing wood chip to prepare active carbon with high specific surface area to overcome above the deficiencies in the prior art, improving gac specific surface area.
Technical scheme of the present invention is as follows:
Utilize wood chip to prepare a method for active carbon with high specific surface area, comprise the following steps:
Step one, is placed in reflux by wood chip, adds the mixed solution of ethyl acetate and dehydrated alcohol, reflux 120-150 minute, filters and obtains solid mixture;
Step 2, carbonizes solid mixture in charring furnace, obtains carbonized material;
Step 3, immerses carbonized material in hydrochloric acid soln, keeps 50-80 minute, filters, and washed with de-ionized water 3-5 time of the solids after filtration, obtains material one;
Step 4, gets material one and triethylamine and 2-methyl isophthalic acid, and 3-divinyl reacts, and filters, and is dipped in hydrochloric acid soln, keeps 40-50 minute, filter the solids after filtering, obtain material two;
Step 5, uses washed with de-ionized water 3-5 time by material two, then under the condition of nitrogen protection, is warming up to 200-250 DEG C, keeps 100-120 minute, is down to room temperature, obtains gac.
The described wood chip that utilizes prepares the method for active carbon with high specific surface area, in step one ethyl acetate and dehydrated alcohol mixed solution in the mass ratio of ethyl acetate and dehydrated alcohol be 10:15-20.
The described wood chip that utilizes prepares the method for active carbon with high specific surface area, and in step one, the quality of mixed solution is 2-4 times of wood chip quality.
The described wood chip that utilizes prepares the method for active carbon with high specific surface area, and the condition carbonized in step 2 is carbonization temperature 700-800 DEG C, carbonization time 200-250 minute.
The described wood chip that utilizes prepares the method for active carbon with high specific surface area, and in step 3, the mass concentration of hydrochloric acid is 5-10%.
The described wood chip that utilizes prepares the method for active carbon with high specific surface area, and material one and triethylamine and 2-methyl isophthalic acid in step 4, the mass ratio of 3-divinyl is 10:1-3:0.2-0.5.
The described wood chip that utilizes prepares the method for active carbon with high specific surface area, and in step 4, the mass concentration of hydrochloric acid soln is 5-10%.
The described wood chip that utilizes prepares the method for active carbon with high specific surface area, and material one and triethylamine and 2-methyl isophthalic acid in step 4,3-divinyl reaction conditions for stir 30-50 minute under 40 DEG C of conditions.
The gac specific surface area that preparation method provided by the invention obtains reaches 3980m
2/ more than g, adsorptive value reaches more than 1450mg, and ash content is lower simultaneously, can meet the requirement of absorption better.
Embodiment:
Embodiment 1
Utilize wood chip to prepare a method for active carbon with high specific surface area, comprise the following steps:
Step one, is placed in reflux by wood chip 1250g, adds the mixed solution of ethyl acetate 1000g and dehydrated alcohol 1500g, reflux 120 minutes, filters and obtains solid mixture;
Step 2, carbonizes solid mixture in charring furnace, carbonization temperature 700 DEG C, and carbonization time 200 minutes, obtains carbonized material;
Step 3, carbonized material being immersed mass concentration is in the hydrochloric acid soln of 5%, keeps 50 minutes, filters, and the washed with de-ionized water 3 times of the solids after filtration, obtains material one;
Step 4, gets material one 200g and 20g triethylamine and 4g2-methyl isophthalic acid, and 3-divinyl stirring reaction 30 minutes under 40 DEG C of conditions, filters, and it is in the hydrochloric acid soln of 5% that the solids after filtering is dipped in mass concentration, and keeps 40 minutes, filtration, obtains material two;
Step 5, uses washed with de-ionized water 3 times, then under the condition of nitrogen protection, is warming up to 200 DEG C by material two, keep 100 minutes, be down to room temperature, obtain gac.
Embodiment 2
Utilize wood chip to prepare a method for active carbon with high specific surface area, comprise the following steps:
Step one, is placed in reflux by 1500g wood chip, adds the mixed solution of 1500g ethyl acetate and 2500g dehydrated alcohol, reflux 120-150 minute, filters and obtains solid mixture;
Step 2, carbonizes solid mixture in charring furnace, carbonization temperature 750 DEG C, and carbonization time 220 minutes, obtains carbonized material;
Step 3, carbonized material being immersed mass concentration is in the hydrochloric acid soln of 6%, keeps 60 minutes, filters, and the washed with de-ionized water 4 times of the solids after filtration, obtains material one;
Step 4, gets material one 200g and 40g triethylamine and 6g2-methyl isophthalic acid, and 3-divinyl stirring reaction 35 minutes under 40 DEG C of conditions, filters, and it is in the hydrochloric acid soln of 6% that the solids after filtering is dipped in mass concentration, and keeps 43 minutes, filtration, obtains material two;
Step 5, uses washed with de-ionized water 3 times, then under the condition of nitrogen protection, is warming up to 210 DEG C by material two, keep 105 minutes, be down to room temperature, obtain gac.
Embodiment 3
Utilize wood chip to prepare a method for active carbon with high specific surface area, comprise the following steps:
Step one, is placed in reflux by wood chip 1500g, adds the mixed solution of 1800g ethyl acetate and 3200g dehydrated alcohol, reflux 140 minutes, filters and obtains solid mixture;
Step 2, carbonizes solid mixture in charring furnace, carbonization temperature 780 DEG C, and carbonization time 230 minutes, obtains carbonized material;
Step 3, carbonized material being immersed mass concentration is in the hydrochloric acid soln of 8%, keeps 70 minutes, filters, and the washed with de-ionized water 4 times of the solids after filtration, obtains material one;
Step 4, gets material one 250g and 50g triethylamine and 8g2-methyl isophthalic acid, and 3-divinyl reacts 40 minutes under 40 DEG C of conditions, filters, and then the solids after filtration being dipped in mass concentration is in the hydrochloric acid soln of 8%, keeps 45 minutes, filters, obtains material two;
Step 5, uses washed with de-ionized water 5 times, then under the condition of nitrogen protection, is warming up to 240 DEG C by material two, keep 110 minutes, be down to room temperature, obtain gac.
Plastics 4
Utilize wood chip to prepare a method for active carbon with high specific surface area, comprise the following steps:
Step one, is placed in reflux by wood chip 1500g, adds the mixed solution of 2000g ethyl acetate and 4000g dehydrated alcohol, reflux 150 minutes, filters and obtains solid mixture;
Step 2, carbonizes solid mixture in charring furnace, carbonization temperature 800 DEG C, and carbonization time 250 minutes, obtains carbonized material;
Step 3, carbonized material being immersed mass concentration is in the hydrochloric acid soln of 10%, keeps 80 minutes, filters, and the washed with de-ionized water 5 times of the solids after filtration, obtains material one;
Step 4, gets material one 250g and 75g triethylamine and 12.5g2-methyl isophthalic acid, 3-divinyl stirring reaction 50 minutes under 40 DEG C of conditions, filter, it is in the hydrochloric acid soln of 10% that the solids after filtration is dipped in mass concentration, keeps 50 minutes, filter, obtain material two;
Step 5, uses washed with de-ionized water 5 times, then under the condition of nitrogen protection, is warming up to 250 DEG C by material two, keep 120 minutes, be down to room temperature, obtain gac.
Carry out performance test to the gac that above embodiment prepares, result is as follows:
Project | Specific surface area/m 2/g | Ash content/% | Adsorptive value/mg |
Embodiment 1 | 3980 | 2.98 | 1450 |
Embodiment 2 | 4230 | 2.86 | 1480 |
Embodiment 3 | 4560 | 2.85 | 1550 |
Embodiment 4 | 4370 | 2.82 | 1530 |
As can be seen from above test-results, the gac specific surface area that preparation method provided by the invention obtains reaches 3980m
2/ more than g, adsorptive value reaches more than 1450mg, and ash content is lower simultaneously, therefore, it is possible to meet the requirement of absorption better.
Claims (8)
1. utilize wood chip to prepare a method for active carbon with high specific surface area, it is characterized in that, comprise the following steps:
Step one, is placed in reflux by wood chip, adds the mixed solution of ethyl acetate and dehydrated alcohol, reflux 120-150 minute, filters and obtains solid mixture;
Step 2, carbonizes solid mixture in charring furnace, obtains carbonized material;
Step 3, immerses carbonized material in hydrochloric acid soln, keeps 50-80 minute, filters, and washed with de-ionized water 3-5 time of the solids after filtration, obtains material one;
Step 4, gets material one and triethylamine and 2-methyl isophthalic acid, and 3-divinyl reacts, and filters, and is dipped in hydrochloric acid soln, keeps 40-50 minute, filter the solids after filtering, obtain material two;
Step 5, uses washed with de-ionized water 3-5 time by material two, then under the condition of nitrogen protection, is warming up to 200-250 DEG C, keeps 100-120 minute, is down to room temperature, obtains gac.
2. the method utilizing wood chip to prepare active carbon with high specific surface area according to claim 1, is characterized in that, in step one ethyl acetate and dehydrated alcohol mixed solution in the mass ratio of ethyl acetate and dehydrated alcohol be 10:15-20.
3. the method utilizing wood chip to prepare active carbon with high specific surface area according to claim 1, is characterized in that, in step one, the quality of mixed solution is 2-4 times of wood chip quality.
4. the method utilizing wood chip to prepare active carbon with high specific surface area according to claim 1, is characterized in that, the condition carbonized in step 2 is carbonization temperature 700-800 DEG C, carbonization time 200-250 minute.
5. the method utilizing wood chip to prepare active carbon with high specific surface area according to claim 1, is characterized in that, in step 3, the mass concentration of hydrochloric acid is 5-10%.
6. the method utilizing wood chip to prepare active carbon with high specific surface area according to claim 1, is characterized in that, material one and triethylamine and 2-methyl isophthalic acid in step 4, the mass ratio of 3-divinyl is 10:1-3:0.2-0.5.
7. the method utilizing wood chip to prepare active carbon with high specific surface area according to claim 1, is characterized in that, in step 4, the mass concentration of hydrochloric acid soln is 5-10%.
8. the method utilizing wood chip to prepare active carbon with high specific surface area according to claim 1, is characterized in that, material one and triethylamine and 2-methyl isophthalic acid in step 4,3-divinyl reaction conditions for stir 30-50 minute under 40 DEG C of conditions.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101759181A (en) * | 2009-12-15 | 2010-06-30 | 李广朝 | Method for producing activated carbon for super capacitors |
CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
CN102153082A (en) * | 2011-04-25 | 2011-08-17 | 福建省将乐县乐洪活性炭有限公司 | Method for preparing wood activated carbon by phosphoric acid method |
CN103084187A (en) * | 2012-12-17 | 2013-05-08 | 常州大学 | Carbon-based solid acid and preparation method thereof |
CN104140099A (en) * | 2014-08-18 | 2014-11-12 | 福建师范大学 | Method for preparing bio-based active carbon by using basic ionic liquid as activator |
-
2015
- 2015-09-30 CN CN201510642974.4A patent/CN105197929A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101759181A (en) * | 2009-12-15 | 2010-06-30 | 李广朝 | Method for producing activated carbon for super capacitors |
CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
CN102153082A (en) * | 2011-04-25 | 2011-08-17 | 福建省将乐县乐洪活性炭有限公司 | Method for preparing wood activated carbon by phosphoric acid method |
CN103084187A (en) * | 2012-12-17 | 2013-05-08 | 常州大学 | Carbon-based solid acid and preparation method thereof |
CN104140099A (en) * | 2014-08-18 | 2014-11-12 | 福建师范大学 | Method for preparing bio-based active carbon by using basic ionic liquid as activator |
Non-Patent Citations (1)
Title |
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胡蝶等: "提取条件对竹纤维分级分离的影响", 《生物质化学工程》 * |
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