CN105923633B - The method that content of ashes is reduced during preparing activated carbon with straw - Google Patents
The method that content of ashes is reduced during preparing activated carbon with straw Download PDFInfo
- Publication number
- CN105923633B CN105923633B CN201610252828.5A CN201610252828A CN105923633B CN 105923633 B CN105923633 B CN 105923633B CN 201610252828 A CN201610252828 A CN 201610252828A CN 105923633 B CN105923633 B CN 105923633B
- Authority
- CN
- China
- Prior art keywords
- straw
- activated carbon
- content
- phosphoric acid
- ashes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Carbon And Carbon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A method of it reducing content of ashes during preparing activated carbon with straw, belongs to the preparation field of activated carbon.Activator prepares activated carbon the purpose of the present invention is using straw as raw material, being with phosphoric acid, and can be greatly lowered content of ashes prepare activated carbon with straw during reduce the method for content of ashes.The present invention interception by 60 mesh sieve pore by cannot pass through the straw powder of 80 mesh sieve pores；It under the conditions of in autoclave with 260 300 DEG C of temperature, reacts 12 hours, is centrifuged 3 minutes with 3000 revs/min of rotating speed after cooling, obtain filtrate and filter residue；Place into Muffle furnace, priming reaction 1 hour, that is, prepare the activated carbon of content of ashes 3.2 8.5% at 500 DEG C.Present invention process is simple, by the adjustment to process conditions, can greatly reduce the content of ash content in activated carbon, to improve the quality of activated carbon.
Description
Technical field
The invention belongs to the preparation fields of activated carbon.
Background technology
Activated carbon is a kind of special porous carbon material, and pore structure is flourishing, has that adsorption capacity is strong, chemical property is steady
It is fixed, using after failure the advantages that regenerating easily.Activated carbon is widely used as the adsorbent and catalyst carrier of excellent properties.
Traditional activated carbon preparation be the natural resources such as coal and oil using the wood material of natural plant kind and mineral substance as raw material into
Prepared by row, increasingly severe with environment and ecological problem, activated carbon raw material sources are limited, price also continuous rise.
By-product of the straw as agricultural production, resource are very abundant.For a long time, China various regions rural area is generally to straw
Burning disposal is carried out, thus severe air is brought to pollute, especially in recent years, China takes place frequently large-scale depth haze, solves rice
The agricultural wastes such as grass burn the environmental pollution brought and have been very urgent.Active raw material of wood-charcoal is prepared using abandoned biomass such as straw
Material is the effective way for solving current quagmire, and the preparation research of the biomass-based activated carbon of straw meets the principle of Green Chemistry, and
The development of renewable chemicals and material industry can be pushed significantly.
Invention content
The purpose of the present invention is using straw as raw material, be that activator prepares activated carbon, and can be greatly lowered with phosphoric acid
Content of ashes prepares the method that content of ashes is reduced during activated carbon with straw.
Step of the present invention is：
(1) it goes the straw of root and fringe to be cut into segment to be put into pulverizer after washing dedusting drying and wear into fine powder, mistake
Sieve, interception by 60 mesh sieve pore by cannot pass through the straw powder of 80 mesh sieve pores；
(2) 10 g of rice straw powder end in step (1) are taken, are mixed with the phosphoric acid of 150-200 mL mass percentage concentrations 85%
It is even, it is placed in Stirring autoclave, under the conditions of 260-300 DEG C of temperature, is reacted 1-2 hour, with 3000 revs/min after cooling down
The rotating speed of clock centrifuges 3 minutes, obtains filtrate and filter residue；
(3) filter residue is placed in porcelain crucible, closes crucible cover starvation, be put into Muffle furnace, priming reaction 1 at 500 DEG C
Hour；Taking-up washing, filtering, dry, smashing are screened to 100 mesh, that is, prepare the activated carbon of content of ashes 3.2-8.5%.
Present invention process is simple, by the adjustment to process conditions, can greatly reduce the content of ash content in activated carbon,
To improve the quality of activated carbon.Its advantage is that：
It is pre-processed using phosphoric acid high temperature hydro-thermal method, prepares the biomass-based activated carbon of straw of content of ashes 3.2-8.5%,
The ash content in straw is significantly reduced, and then the absorption property of the biomass-based activated carbon of straw can be improved；
The phosphoric acid for being immersed in straw surface can be directly as activator, and activity can be prepared by no longer needing to add other activators
Charcoal reduces cost.
Straw abandoned biomass is made full use of, is turned waste into wealth, there is good industrial prospect.
Specific implementation mode
Step of the present invention is：
(1) it goes the straw of root and fringe to be cut into segment to be put into pulverizer after washing dedusting drying and wear into fine powder, mistake
Sieve, interception by 60 mesh sieve pore by cannot pass through the straw powder of 80 mesh sieve pores；
(2) 10 g of rice straw powder end in step (1) are taken, are mixed with the phosphoric acid of 150-200 mL mass percentage concentrations 85%
It is even, it is placed in Stirring autoclave, under the conditions of 260-300 DEG C of temperature, is reacted 1-2 hour, with 3000 revs/min after cooling down
The rotating speed of clock centrifuges 3 minutes, obtains filtrate and filter residue；
(3) filter residue is placed in porcelain crucible, closes crucible cover starvation, be put into Muffle furnace, priming reaction 1 at 500 DEG C
Hour；Taking-up washing, filtering, dry, smashing are screened to 100 mesh, that is, prepare the activated carbon of content of ashes 3.2-8.5%.
The present invention is described in further details below：
The present invention includes the following steps：
(1) it goes the straw of root and fringe to be cut into segment to be put into pulverizer after washing dedusting drying and wear into fine powder, mistake
Sieve, interception by 60 mesh sieve pore by cannot by the straw powder of 80 mesh sieve pores for lower step experiment.
(2) 10 g of rice straw powder end in step (1) are taken, with 150-200 mL (solid-to-liquid ratios 1:15-1:20) mass percentage concentration
85% phosphoric acid is uniformly mixed, and is placed in Stirring autoclave（500 revs/min of rotating speed）, in 260-300 DEG C of condition of temperature
Under, it reacts 1-2 hours, is centrifuged 3 minutes with 3000 revs/min of rotating speed after cooling, obtain filtrate and filter residue.
(3) filter residue is placed in porcelain crucible, closes crucible cover starvation, be put into Muffle furnace, priming reaction 1 at 500 DEG C
Hour.Taking-up washing, filtering, dry, smashing are screened to 100 mesh, that is, prepare the activated carbon of content of ashes 3.2-8.5%.
(4) in activated carbon sample the assay method of content of ashes with reference to GB/T 12496.3-1999.By dried work
Property charcoal sample be placed in calcination to the porcelain crucible of constant weight, keep crucible opening-wide state, be put into temperature and be no more than 300 DEG C of Muffle
In stove, 650 DEG C of ashing are warming up to constant weight, content of ashes is indicated with the percentage of the quality of gained ash and original sample quality.
Phosphoric acid is widely used in the preparation process of activated carbon as activator, usually mixes phosphoric acid in proportion with raw material
Close, Muffle furnace high temperature heat, make charing, activation be carried out at the same time or branch carry out, in activation process, the volatilization in raw material
Property ingredient is discharged in the form of water, carbon dioxide, methane, carbon monoxide etc., while the production of tar is inhibited, and phosphoric acid has removing
Moisture content, oxidation and etching effect, finally prepare activated carbon.
But the content of ashes in straw, up to 10-15%, the ash content in straw is the mineral member in rice-straw fibre raw material
Element exists in the form of inorganic salts and oxide, mainly potassium, sodium, calcium, magnesium, sulphur, phosphorus, the oxide of silicon, sulfate and phosphoric acid
The forms such as salt, the ash content in straw is mainly silica, accounts for 60% of content of ashes or more.Since content of ashes is high in straw,
Therefore high ash content is also contained by activated carbon prepared by straw, affect the absorption property of activated carbon.
The process of the present invention is pre-processed using the phosphoric acid high temperature hydro-thermal method of mass fraction 85%, in 260-300 DEG C of high-temperature water
Under heat condition, the solid-to-liquid ratio 1 of straw and phosphoric acid:15-1:20, so that phosphoric acid is fully reacted with the ash content in straw.Reaction principle is such as
Under：
Sylvite and sodium salt in ash content are dissolved in the water phase of 85% phosphoric acid solution as soluble-salt.Phosphoric acid is heated to 245 DEG C
When above, intermolecular dehydration forms pyrophosphoric acid.
2H3PO4→H4P2O7+H2O
Silica and pyrophosphoric acid in ash content react the heteropoly acid to form silicon phosphoric acid and are dissolved in 85% phosphoric acid solution.
SiO2+ H4P2O7→H2Si (PO4)2 +H2O
After pretreatment, centrifuges filter residue and filtrate, the phosphoric acid for being immersed in straw surface can be not necessarily to directly as activator
Add again other activators can prepare content of ashes 3.2-8.5% the biomass-based activated carbon of straw.
Embodiment 1：It goes the straw of root and fringe to be cut into segment to be put into pulverizer after washing dedusting drying and wear into fine powder,
Sieving, interception by 60 mesh sieve pore by cannot by the straw powder of 80 mesh sieve pores for lower step experiment.Take 10 g of straw powder
Without the preprocessing process of the hot method of peroxophosphoric acid high-temperature water, mixed with the phosphoric acid of 40 mL mass percentage concentrations 85% in porcelain crucible
It is even, crucible cover starvation is closed, is put into Muffle furnace, priming reaction 1 hour at 500 DEG C.Take out washing, filtering, dry, powder
Essence is screened to 100 mesh, prepares the activated carbon that content of ashes is 21.6%.
Embodiment 2：It goes the straw of root and fringe to be cut into segment to be put into pulverizer after washing dedusting drying and wear into fine powder.
Sieving, interception by 60 mesh sieve pore by cannot by the straw powder of 80 mesh sieve pores for lower step experiment.10 g of straw powder is taken,
With 150 mL (solid-to-liquid ratios 1:15) the phosphoric acid mixing of mass percentage concentration 85%, is placed in Stirring autoclave（Rotating speed 500
Rev/min）, under the conditions of 240 DEG C of temperature, react 1 hour, centrifuged 3 minutes with 3000 revs/min of rotating speed after cooling.
Filter residue is placed in porcelain crucible, starvation on crucible cover is closed, is put into Muffle furnace, priming reaction 1 hour at 500 DEG C.It takes out
Washing, filtering, dry, smashing are screened to 100 mesh, prepare the activated carbon that content of ashes content is 16.1%.
Embodiment 3-11：According to the process conditions listed by table 1, the step of according to embodiment 2, the ash of prepared activated carbon
Point content is also listed in Table 1.
1 embodiment condition table of table
By the overall merit to embodiment 1-11, straw powder is pre-processed through phosphoric acid high temperature hydro-thermal method, that is, controls straw
The phosphoric acid solid-to-liquid ratio of powder and mass percentage concentration 85% is 1:15-1:React 1-2 hours under the conditions of 20,260-300 DEG C, significantly
The ash content in straw is reduced, the biomass-based activated carbon of straw of content of ashes 3.2-8.5% has been prepared.
Claims (1)
1. a kind of preparing the method for reducing content of ashes during activated carbon with straw, it is characterised in that：Its step is：
（1）It goes the straw of root and fringe to be cut into segment to be put into pulverizer after washing dedusting drying and wear into fine powder, be sieved,
（2）Interception by 60 mesh sieve pore by cannot pass through the straw powder of 80 mesh sieve pores；
（3）10 g of rice straw powder end in step (1) are taken, are uniformly mixed with the phosphoric acid of 150-200 mL mass percentage concentrations 85%, wherein
The solid-to-liquid ratio of straw powder and phosphoric acid is 1:15-1:20, it is placed in Stirring autoclave, 500 revs/min of reaction kettle rotating speed
Clock reacts 1-2 hour under the conditions of 260-300 DEG C of temperature, it is cooling after with 3000 revs/min of rotating speed centrifugation 3 minutes,
Obtain filtrate and filter residue；
Reaction principle is as follows：
Sylvite and sodium salt in ash content are dissolved in the water phase of 85% phosphoric acid solution as soluble-salt；Phosphoric acid is heated to 245 DEG C or more
When, intermolecular dehydration forms pyrophosphoric acid；
2H3PO4→H4P2O7+H2O
Silica and pyrophosphoric acid in ash content react the heteropoly acid to form silicon phosphoric acid and are dissolved in 85% phosphoric acid solution；
SiO2+ H4P2O7→H2Si (PO4)2 +H2O
（4）After pretreatment, centrifuges filter residue and filtrate, the phosphoric acid for being immersed in straw surface can be not necessarily to directly as activator
Other activators are added again；Filter residue is placed in porcelain crucible, crucible cover starvation is closed, is put into Muffle furnace, 500 DEG C of whens activate
Reaction 1 hour；Take out washing, filtering, it is dry, smash and be screened to 100 mesh, you can prepare content of ashes 3.2-8.5% straw
Biomass-based activated carbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610252828.5A CN105923633B (en) | 2016-04-22 | 2016-04-22 | The method that content of ashes is reduced during preparing activated carbon with straw |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610252828.5A CN105923633B (en) | 2016-04-22 | 2016-04-22 | The method that content of ashes is reduced during preparing activated carbon with straw |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105923633A CN105923633A (en) | 2016-09-07 |
| CN105923633B true CN105923633B (en) | 2018-10-16 |
Family
ID=56839787
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610252828.5A Expired - Fee Related CN105923633B (en) | 2016-04-22 | 2016-04-22 | The method that content of ashes is reduced during preparing activated carbon with straw |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105923633B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107043162A (en) * | 2017-06-26 | 2017-08-15 | 苏州科技大学 | A kind of method of straw activated carbon reinforced anaerobic sludge Combined Processing azo dye wastewater |
| CN112047338A (en) * | 2020-10-21 | 2020-12-08 | 南京正森环保科技有限公司 | Method for preparing wood activated carbon with ultralow phosphoric acid consumption |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891189A (en) * | 2010-08-13 | 2010-11-24 | 宁乡县亮之星米业有限公司 | Method for preparing coal gas, top-grade active carbon, water glass and silicate phosphate from rice hulls |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MX2009008786A (en) * | 2007-02-14 | 2009-08-25 | Univ Kentucky Res Foundation I | Methods of forming activated carbons. |
| CN102502621B (en) * | 2011-11-28 | 2014-01-01 | 中南大学 | Post-treatment process for preparing super-capacitor active carbon with super-low ash content |
| CN104085890B (en) * | 2014-07-15 | 2016-05-11 | 李文军 | Maize straw carbon fiber production method |
| CN104724703A (en) * | 2015-03-20 | 2015-06-24 | 福州大学 | Method for preparing adsorptive activated carbon from Musaceae plants |
| CN105439144A (en) * | 2015-11-18 | 2016-03-30 | 福建翔丰华新能源材料有限公司 | Method for preparing high-performance activated carbon |
| CN105480973A (en) * | 2015-12-14 | 2016-04-13 | 河北工业大学 | Method for efficiently preparing cotton based mesoporous activated carbon fiber |
| CN105399872B (en) * | 2015-12-22 | 2018-06-15 | 齐鲁工业大学 | A kind of method and application using Jujun grasses Preparation of Activated Carbon with Lignin |
-
2016
- 2016-04-22 CN CN201610252828.5A patent/CN105923633B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891189A (en) * | 2010-08-13 | 2010-11-24 | 宁乡县亮之星米业有限公司 | Method for preparing coal gas, top-grade active carbon, water glass and silicate phosphate from rice hulls |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105923633A (en) | 2016-09-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103121682B (en) | Method for preparing high-specific-surface-area activated carbon from tobacco stalks | |
| CN102745879B (en) | Sludge-based adsorbent used for desulfurization and demercuration of flue-gas and preparation method thereof | |
| CN104941589A (en) | Preparation method of porous biological carbon heavy metal adsorbing material based on cotton straw | |
| WO2015106720A1 (en) | Method for producing super activated charcoal from biomass power plant ash | |
| CN106904589A (en) | A kind of hydro-thermal method prepares method and the application of bagasse Carbon Materials | |
| CN107235759B (en) | Carbon-phosphorus compound fertilizer and method for preparing carbon-phosphorus compound fertilizer by using sludge | |
| CN106698418A (en) | Self-templated fibrous biomass-based porous carbon material and preparation method and application thereof | |
| CN103288080B (en) | A kind ofly prepare the ecological carbon method that mesoporous is high, adsorptivity is strong | |
| CN102417179B (en) | Preparation method of activated carbon material for electrochemical capacitor | |
| CN106732375A (en) | A kind of preparation method and applications of clay mineral modification biological charcoal | |
| CN103496700A (en) | Method for preparing active carbon from pyrolysis residues of cedarwood sawdust | |
| CN106115699A (en) | Zinc oxide method prepares activated carbon | |
| CN105923633B (en) | The method that content of ashes is reduced during preparing activated carbon with straw | |
| CN106563505A (en) | Catalyst for coal gasification, preparation method and application thereof | |
| CN108569836A (en) | A kind of the dehydration stabilization method and device of chromium-bearing sludge | |
| CN112705166A (en) | Preparation method and application of ammonia water modified eucalyptus activated carbon adsorbent | |
| CN108929737A (en) | Biomass solid clean fuel and its preparation method and application | |
| CN103785353A (en) | Method for preparing composite activated carbon-zeolite material from coal gangue | |
| CN102424383B (en) | Method for preparing mesoporous carbon material for electrochemical capacitor | |
| CN104801306B (en) | A kind of powder activity Pd/carbon catalyst prepared using turf as raw material and preparation method | |
| CN102838112A (en) | Preparation method of activated carbon | |
| CN113750961A (en) | Carbon dioxide adsorbent and preparation method thereof | |
| CN113522240A (en) | Method for preparing desulfurization activated carbon by solid-phase hydrothermal modified biochar | |
| CN109319782A (en) | A kind of preparation method of sodium lignin sulfonate/polystyrene-based activated carbon microballon | |
| CN102247805B (en) | Novel active carbon and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20181016 |