CN104176735A - Method for preparing Chinese soapberry activated carbon by using phosphorus-containing inorganic acid as activator - Google Patents
Method for preparing Chinese soapberry activated carbon by using phosphorus-containing inorganic acid as activator Download PDFInfo
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- CN104176735A CN104176735A CN201410405497.5A CN201410405497A CN104176735A CN 104176735 A CN104176735 A CN 104176735A CN 201410405497 A CN201410405497 A CN 201410405497A CN 104176735 A CN104176735 A CN 104176735A
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- chinese soapberry
- acid
- activated carbon
- activator
- inorganic phosphor
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Abstract
The invention relates to a method for preparing Chinese soapberry activated carbon by using phosphorus-containing inorganic acid as an activator. The preparation method comprises the following steps: 1) drying Chinese soapberry kernels/shells and peel residues in air, pulverizing, washing with an alcoholic solution, and filtering for later use; 2) putting the raw material in a microwave reactor, introducing N2, regulating microwave power and carbonization temperature, and keeping the temperature for carbonization to obtain a carbonization material; 3) mixing the carbonization material with a phosphorus-containing inorganic acid composite activator, adding distilled water, drying after 2 hours, quickly adding into furnace temperature in a N2 protective atmosphere to be activated, cooling and taking out; and 4) washing the obtained activated carbon with hydrochloric acid, washing with water to a neutral state, and drying to obtain the powdery activated carbon finished product. The specific area of the Chinese soapberry activated carbon is 1000-2000 m<2>/g, and the BJH mesopore is 500-800 m<2>/g. The Chinese soapberry activated carbon has the advantages of developed mesopore, reasonable pore structure distribution, moderate apparent density, uniform particle density, stable performance and high adsorption capacity.
Description
Technical field
The invention belongs to forest chemical technical field, be specifically related to a kind of method of preparing Seed of Chinese Soapberry gac taking inorganic phosphor-contained acid as activator.
Background technology
China is large agricultural country, produces every year a large amount of agriculture and forestry organic waste materials, as agricultural crop straw, agricultural processing waste, human and animal excreta etc.China mainly uses two aspects to the treatment process of agriculture and forestry organic waste material at present: the one, burn, but a large amount of dust and the CO that after burning, produce
2bring sizable harm Deng a pollutent atmospheric environment; The 2nd, carry out compost, compost need to take a large amount of soils, because organic substance decomposing thoroughly will not produce a large amount of odorous substances such as lower fatty acid and sulfocompound, affects surrounding enviroment.How effectively utilizing agriculture and forestry organic waste material is inevitable problem in China's industrial and agricultural development process.
The conventional activator of preparing gac has H
3pO
4, KOH, ZnCl etc.H
3pO
4gentleer as activator reaction, relatively little to equipment corrosion, but the specific surface area of the gac of preparation is relatively little; KOH can prepare excellent active carbon with high specific surface area as activator, but the alkali steam and the alkali spittle that produce when priming reaction are larger to the infringement of equipment and environment; ZnCl is large as activator consumption, and the rate of recovery is low, and the waste water and gas of generation works the mischief to environment.
Hou Chaohui (a kind of preparation method of Mesoporous Carbon Materials. the patent No.: CN200910043230.5), Zhang Rongle (a kind of continuous production method of active carbon with high specific surface area. the patent No.: 200610098623.2), Tong Shitang (a kind of mesoporous activated carbon and preparation method thereof. the patent No.: 200810186027.9) and etc. in succession preparation technology and activator have been carried out to certain improvement, but the activation dosage using is larger, stronger to equipment corrosion, effect is all not ideal enough.Phosphatase reaction condition is relatively gentle, and relatively little to the corrodibility of equipment, processing method is simple, be widely used by industry, but single activator is difficult to effectively control gac ground structure, for this reason, take that multiple actives is composite can reasonably control gac ground pore structure.Meanwhile, the process of activation also has a great impact gac ground pore structure.
Seed of Chinese Soapberry is as a kind of energy seeds, planted on a large scale in the whole nation, Seed of Chinese Soapberry fruit has left a large amount of residues after extracting biodiesel raw material oil, Seed of Chinese Soapberry residue contains abundant carbon source, it is the important source material source of gac, at present, there is not yet taking Seed of Chinese Soapberry fruit as raw material, prepare the report of Seed of Chinese Soapberry gac taking inorganic phosphor-contained acid as activator.
Summary of the invention
The object of this invention is to provide a kind of taking Seed of Chinese Soapberry residue as raw material, prepare the method for Seed of Chinese Soapberry gac taking inorganic phosphor-contained acid as activator, simple, avoid the wasting of resources, resource is utilized effectively.
The concrete steps that technical scheme of the present invention is taked are as follows:
(1) raw materials pretreatment
Seed of Chinese Soapberry nucleocapsid and pericarp residue are dried, through pulverizing, alcoholic solution washing 3～8 times, filter for subsequent use.
(2) carbonization
The raw material that step (1) is handled well is put into microwave reactor, passes into N
2, modulated microwave power is that 1000～2000W, carbonization temperature are 500～700 DEG C, insulation carbonization 100～300min obtains carbonized material.
(3) activation
The carbonized material that step (2) is obtained mixes in mass ratio with inorganic phosphor-contained sour composite activating agent, and adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 DEG C, at N
2protection is lower, and to drop into fast furnace temperature be activation insulation 250-300min in the atmosphere furnace of 880 DEG C～900 DEG C, is cooled to room temperature and takes out.
(4) aftertreatment:
By the gac preparing through salt acid elution, be washed to neutrality, dry after obtain powdered active carbon finished product.
The ethanolic soln that alcoholic solution mass concentration described in step of the present invention (1) is 50%-99%
Inorganic phosphor-contained acid activators described in step of the present invention (3) is two kinds or several composition in phosphoric acid, tetra-sodium, metaphosphoric acid, polyphosphoric acid.
The mass ratio of the carbonized material described in step of the present invention (3) and inorganic phosphor-contained sour composite activating agent is 1:1-5.
The Seed of Chinese Soapberry gac specific surface area that the present invention makes is 1000-2000m
2/ g, BJH mesopore are 500-800m
2/ g.Have flourishing mesopore, pore texture distributes rationally, apparent density is moderate, pellet density is even, and stable performance, has strong adsorptive power.Processing unit of the present invention is simple, is easy to scale operation, and abundant raw material, cheap, market outlook are wide.
Method of the present invention is also suitable for the gac of preparing as raw material taking other biological material.
Embodiment
Be below several specific embodiment of the present invention, further illustrate the present invention, but the present invention be not limited only to this.
Embodiment 1
The Seed of Chinese Soapberry residue pulverizing of 100g, the ethanolic soln through 50% are washed 8 times, after oven dry, put into microwave reactor, pass into N
2, modulated microwave power is 1300W, at 500 DEG C, carbonization 300min obtains carbonized material.
The carbonized material 20g obtaining is mixed with the phosphoric acid of 10g, the tetra-sodium of 20g, and adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 DEG C, at N
2protection is lower, and to drop into fast furnace temperature be activation insulation 300min in the atmosphere furnace of 880 DEG C-890 DEG C, cooling through salt acid elution, be washed to neutrality, obtain powdered active carbon finished product after drying.Prepared gac BET specific surface area is 1566m
2/ g, in BJH, pore specific surface area is 725m
2/ g.
Embodiment 2
The Seed of Chinese Soapberry residue pulverizing of 100g, the ethanolic soln through 60% are washed 5 times, after oven dry, put into microwave reactor, pass into N
2, modulated microwave power is 1500W, at 600 DEG C, carbonization 200min obtains carbonized material.
The carbonized material 20g obtaining is mixed with the phosphoric acid of 10g, the metaphosphoric acid of 10g, the polyphosphoric acid of 10g, and adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 DEG C, at N
2protection is lower, and to drop into fast furnace temperature be activation insulation 290min in the atmosphere furnace of 880 DEG C-900 DEG C, cooling through salt acid elution, be washed to neutrality, obtain powdered active carbon finished product after drying.Prepared gac BET specific surface area is 1533m
2/ g, in BJH, pore specific surface area is 672m
2/ g.
Embodiment 3
The Seed of Chinese Soapberry residue pulverizing of 100g, the ethanolic soln through 80% are washed 3 times, after oven dry, put into microwave reactor, pass into N
2, modulated microwave power is 2000W, at 700 DEG C, carbonization 100min obtains carbonized material.
The carbonized material 20g obtaining is mixed with the tetra-sodium of 20g, the metaphosphoric acid of 5g, the polyphosphoric acid of 20g, and adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 DEG C, at N
2protection is lower, and to drop into fast furnace temperature be activation insulation 260min in the atmosphere furnace of 895 DEG C-900 DEG C, cooling through salt acid elution, be washed to neutrality, obtain powdered active carbon finished product after drying.Prepared gac BET specific surface area is 1394m
2/ g, in BJH, pore specific surface area is 589m
2/ g.
Embodiment 4
The Seed of Chinese Soapberry residue pulverizing of 100g, the ethanolic soln through 95% are washed 5 times, after oven dry, put into microwave reactor, pass into N
2, modulated microwave power is 1500W, at 500 DEG C, carbonization 180min obtains carbonized material.
The carbonized material 20g obtaining is mixed with the phosphoric acid of 5g, the tetra-sodium of 3g, the metaphosphoric acid of 20g, the polyphosphoric acid of 60g, and adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 DEG C, at N
2protection is lower, and to drop into fast furnace temperature be activation insulation 300min in the atmosphere furnace of 880 DEG C-885 DEG C, cooling through salt acid elution, be washed to neutrality, obtain powdered active carbon finished product after drying.Prepared gac BET specific surface area is 1007m
2/ g, in BJH, pore specific surface area is 508m
2/ g.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. a method of preparing Seed of Chinese Soapberry gac taking inorganic phosphor-contained acid as activator, is characterized in that:
1) Seed of Chinese Soapberry nucleocapsid and pericarp residue are dried, through pulverizing, alcoholic solution washing 3～8 times, filter for subsequent use;
2) by step 1) raw material handled well puts into microwave reactor, passes into N
2, modulated microwave power is that 1000～2000W, carbonization temperature are 500～700 DEG C, insulation carbonization 100～300min obtains carbonized material;
3) by step 2) carbonized material that obtains mixes in mass ratio with inorganic phosphor-contained sour composite activating agent, and adding distil water submergence is also stirred after 2h, dry in the constant temperature blast drying ovens of 105 DEG C, at N
2protection is lower, and to drop into fast furnace temperature be activation insulation 250-300min in the atmosphere furnace of 880 DEG C 900 DEG C, is cooled to room temperature and takes out;
4) by the gac preparing through salt acid elution, be washed to neutrality, dry after obtain powdered active carbon finished product.
2. a kind of method of preparing Seed of Chinese Soapberry gac taking inorganic phosphor-contained acid as activator according to claim 1, is characterized in that the ethanolic soln that described alcoholic solution mass concentration is 50%～99%.
3. a kind of method of preparing Seed of Chinese Soapberry gac taking inorganic phosphor-contained acid as activator according to claim 1, is characterized in that described inorganic phosphor-contained acid activators is two kinds or the composition of several arbitrary proportions in phosphoric acid, tetra-sodium, metaphosphoric acid, polyphosphoric acid.
4. a kind of method of preparing Seed of Chinese Soapberry gac taking inorganic phosphor-contained acid as activator according to claim 1, is characterized in that described carbonized material and the mass ratio of inorganic phosphor-contained sour composite activating agent are 1:1～5.
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|---|---|---|---|
| CN201410405497.5A CN104176735A (en) | 2014-08-18 | 2014-08-18 | Method for preparing Chinese soapberry activated carbon by using phosphorus-containing inorganic acid as activator |
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| CN201410405497.5A CN104176735A (en) | 2014-08-18 | 2014-08-18 | Method for preparing Chinese soapberry activated carbon by using phosphorus-containing inorganic acid as activator |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105559140A (en) * | 2016-02-25 | 2016-05-11 | 云南中烟工业有限责任公司 | Porous material made of Chinese herbal medicine extracted residues and application of porous material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6060424A (en) * | 1995-09-28 | 2000-05-09 | Westvaco Corporation | High energy density carbons for use in double layer energy storage devices |
| US20070021300A1 (en) * | 2003-05-09 | 2007-01-25 | Jean-Pierre Farant | Process for the production of activated carbon |
| CN103896267A (en) * | 2012-12-27 | 2014-07-02 | 福建大青实业有限公司 | Processing technology of shell carrier activated carbon |
| CN103896268A (en) * | 2014-04-08 | 2014-07-02 | 山东大学 | Method for preparing multistage-aperture activated carbon with high specific surface area |
-
2014
- 2014-08-18 CN CN201410405497.5A patent/CN104176735A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6060424A (en) * | 1995-09-28 | 2000-05-09 | Westvaco Corporation | High energy density carbons for use in double layer energy storage devices |
| US20070021300A1 (en) * | 2003-05-09 | 2007-01-25 | Jean-Pierre Farant | Process for the production of activated carbon |
| CN103896267A (en) * | 2012-12-27 | 2014-07-02 | 福建大青实业有限公司 | Processing technology of shell carrier activated carbon |
| CN103896268A (en) * | 2014-04-08 | 2014-07-02 | 山东大学 | Method for preparing multistage-aperture activated carbon with high specific surface area |
Non-Patent Citations (3)
| Title |
|---|
| 李柱来: "《药物化学实验指导》", 31 January 2014, 厦门大学出版社 * |
| 邹节明等: "《现代中成药的药材炮制》", 31 January 2009, 科学出版社 * |
| 郑永娟等: "《植物组织培养》", 29 February 2012, 中国水利水电出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105559140A (en) * | 2016-02-25 | 2016-05-11 | 云南中烟工业有限责任公司 | Porous material made of Chinese herbal medicine extracted residues and application of porous material |
| CN105559140B (en) * | 2016-02-25 | 2019-06-04 | 云南中烟工业有限责任公司 | Residue porous material and application thereof after a kind of Chinese herbal medicine extracts |
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Application publication date: 20141203 |