CN101804988B - Novel method for preparing silicon dioxide and active carbon from rice hull ash - Google Patents
Novel method for preparing silicon dioxide and active carbon from rice hull ash Download PDFInfo
- Publication number
- CN101804988B CN101804988B CN201010162142XA CN201010162142A CN101804988B CN 101804988 B CN101804988 B CN 101804988B CN 201010162142X A CN201010162142X A CN 201010162142XA CN 201010162142 A CN201010162142 A CN 201010162142A CN 101804988 B CN101804988 B CN 101804988B
- Authority
- CN
- China
- Prior art keywords
- rice hull
- hull ash
- sodium carbonate
- filtrate
- silicon dioxide
- 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
Abstract
The invention discloses a novel method for preparing silicon dioxide and active carbon from rice hull ash, in particular relatives to a novel method for preparing silicon dioxide and active carbon from rice hull ash obtained through thermal decomposition of rice hulls. Major raw materials of sodium carbonate react with the rice hull ash after high-temperature decomposition to generate sodium silicate solid, and a soluble glass solution and solid active carbon are obtained after water dissolution, so the one-step completion of the silicon dissolution and activation is realized. The soluble glass solution is carbonized for separating out the silicon dioxide, a sodium carbonate solution is obtained through filtration, and sodium carbonate solid is obtained through crystallization. In the whole preparation process, the sodium carbonate only performs the effect of a catalyst, so sodium carbonate has no consumption, can be in cyclic utilization, reduces the cost, and reduces the waste water discharge. In the silicon dissolution stage, carbon dioxide gas generated by the decomposition of the sodium carbonate is fixed with burning tail gas of the rice hulls to be used as precipitating agents for preparing the silicon dioxide through purification treatment, so the cost is reduced, the greenhouse gas discharge is reduced, and the cyclic utilization of the carbon dioxide is realized.
Description
Technical field
The present invention relates to the novel method that a kind of rice hull ash prepares silicon-dioxide and gac, particularly is raw material with the rice hull ash, and synchronous molten silicon, activation prepare the novel method of carbonic acid gas and yellow soda ash recycle in silicon-dioxide and the gac process.
Background technology
In today of industrialization fast development, the mankind are being faced with the pressure of environment rapid deterioration.Be one of primary problem that solves of people wherein by the caused global warning of Greenhouse effect.In order to tackle Global climate change, national governments all can take economical means, environment protection means, legal means even necessary administration means, the development of restriction high energy consumption, high pollution industry.China's " action target of control greenhouse gas emission " is: realize unit gross domestic product carbon dioxide discharge-reduction 40% to the year two thousand twenty.Mind how you go the road of low-carbon (LC), will strive exactly under the overall goal that keeps socio-economic development, realize that with the cost of minimum carbon intensity reduces discharging target.Low-carbon economy and green growth will become the megatrend of future economy development.Therefore the utilization for biomass and product thereof is a starting point with this target just.
China is the abundantest country of rice husk resource in the world, but utilization ratio is low compared with developed countries, and comprehensive utilization benefit is poor.The patent CN1319033A of the D.K. Stephens invention of the U.S. discloses a kind of rice hull ash that rice husk thermal decomposition is obtained and has carried out the gac that the causticization digestion makes, and its iodine number is at least 650-1000. but the main component silicon in the rice hull ash is not related to.
It is the silica hydrogel that raw material obtains with the rice hull ash that patent CN101348255 discloses, and carries out solvent replacing again, prepares the method for hydrophobic silica aerogel; It is the method for feedstock production aerosil that patent CN1449997 discloses with the rice hull ash; CN1669921 discloses the leaching of rice hull ash process strong alkali aqueous solution, neutralization generation silica hydrosol, the adding silicoorganic compound are handled in colloidal sol, form hydrogel, moisture, the constant pressure and dry of hydrogel in aging, washing, organic solvent replacing water gel, make the method for aerosil; CN1039000 disclose with rice hull ash under the condition of heating, pressurizeing with the technology of caustic soda soln water generation reaction glass and gac; CN1229057 discloses under heating, pressurize, add water condition the technology that rice hull ash and caustic soda is dropped into preparation gac and water glass product in the reactor in 10: 3 ratio; CN1319033 discloses and a kind ofly the rice husk thermal decomposition ash is carried out the causticization digestion has made process of active carbon; CN1756719 discloses rice hull ash and has fed carbonic acid gas precipitation preparation silicon-dioxide through soda boiling filtrate, and the yellow soda ash of generation becomes the sodium hydroxide cyclic utilization method with the calcium oxide reaction regeneration; CN1792789 disclose rice hull ash through pickling, soda boiling, hydrochloric acid be neutralized into gel, dry after high-energy ball milling prepare the method for nano silicon; CN101259964 discloses the method for preparing aerosil with the rice hull ash for the raw material constant pressure and dry; CN101264885 discloses and has utilized rice hull ash to produce alkali lixiviation slag behind the water glass through washing, and to adopt potassium hydroxide be that activator activates; Make the technology of gel powder with high adsorptive gac again through washing, oven dry; CN101391778 discloses rice hull ash has been washed to neutrality, and oven dry back alkali cleaning makes water glass solution, adds metal ion chelation agent, and the auxiliary washing of ultrasonic wave makes the method for high-purity siliceous reinforcing agent; CN101402458 discloses the technology of the alkaline process Processing of Preparation nano silicon of rice hull ash; CN1319033 discloses a kind of rice hull ash that rice husk thermal decomposition is obtained and has carried out the gac that the causticization digestion makes; CN101456555 discloses rice hull ash elder generation's alkali cleaning pickling again, makes soluble glass of high modulus and process of active carbon through re-activation; CN1113216 disclose rice hull ash under the condition of pressurization of heating and soda ash solution in stirred autoclave, carry out chemical reaction, after filtration, cooling, filter, the method for making beating neutralization, filtration, oven dry and hyperthermia drying silicon-dioxide.
In the above patent, partial monopoly utilizes the silicon source in the rice hull ash to prepare water glass, silicon-dioxide separately; Partial monopoly utilizes the carbon source in the rice hull ash to prepare gac separately, rice hull ash is not made full use of.Also have partial monopoly to separate charcoal and silicon-dioxide earlier, the high-temperature activation charcoal prepares gac again, makes that the cost of reaction is too high.And the waste liquid that most patent and reckoning without produces in production process, waste gas are to the pollution of environment.
Summary of the invention
The objective of the invention is to the rice hull ash behind the rice husk thermal decomposition is prepared nano silicon and gac, preparation process is not for producing the low-carbon (LC) friendly process of waste gas, waste residue.
The present invention includes following two steps:
(1) high-temperature fusion activation filter residue prepares gac
Is 1: 1.5～3.0 ratio uniform mixing with rice hull ash, solid sodium carbonate or salt of wormwood in mass ratio, places High Temperature Furnaces Heating Apparatus to be warming up to 850～950 ℃, the constant temperature frit reaction, reclaim tail gas simultaneously, stop heating behind reaction 0.5～2h, be cooled in 100 ℃, be transferred to and be heated to boiling dissolving 0.5～2h in the dissolution kettle, filtering separation filtrate and filter residue, filter residue is washed through diluted acid, washed with water again till the neutrality, filter, drying, pack activated carbon product.
(2) filtrate prepares silicon-dioxide
The filtrate of step (1) is placed reactor, and adjusting temperature is 70～95 ℃, feeds carbon dioxide mix gas in (1), carbonization 1h, ageing 3h filters, the filtrate condensing crystal returns step (1) recycle, filter cake washing, drying, pulverizing, pack silica product.
The invention is characterized in: rice hull ash and yellow soda ash or salt of wormwood heating and melting, discharge carbonic acid gas, mix with the rice husk combustion tail gas, adjusting the carbonic acid gas massfraction is 25～40%, is used for step (2) carburizing reagent, recycle.
The invention is characterized in: filtrate in the step (2), reclaim yellow soda ash or salt of wormwood through condensing crystal, return step (1) recycle.
Advance of the present invention is:
1. generate the water glass solid with the rice hull ash reaction behind the yellow soda ash pyrolytic decomposition, after water-soluble, obtain water glass solution and solid activated carbon, realized that molten silicon, activatory one go on foot and finish.Reduced cost, rice hull ash is fully utilized.
2. molten silicon stage yellow soda ash decomposes the carbon dioxide that produces and mixes with combustion tail gas, through purifying treatment, can be used to prepare the precipitation agent of silicon-dioxide, both avoided the pollution that causes with sour neutralization precipitation in the traditional technology, reduced cost, make full use of again and reclaimed carbonic acid gas, reduced the discharging of greenhouse gases, realized the recycle of carbonic acid gas.
3. yellow soda ash obtains the water glass solid as raw material and rice hull ash reaction, through the water-soluble water glass solution that obtains, separates out silica solid through carbonization again, filters and obtains sodium carbonate solution, and the filtrate crystallization obtains the yellow soda ash solid.Yellow soda ash does not consume in this process, and reusable edible reduces cost, and reduces discharge of wastewater.
4. when preparation silicon-dioxide, need not add other material and prevent that gel from generating, reduce cost, reduce discharge of wastewater.
Below in conjunction with embodiment the present invention is further described:
Embodiment 1: the ratio uniform mixing that with rice hull ash, solid carbonic acid potassium in mass ratio is 1: 1.75, place High Temperature Furnaces Heating Apparatus to be warming up to 700 ℃, stop heating behind the constant temperature frit reaction 1h, be cooled in 100 ℃, be transferred to and be heated to boiling dissolving 1h in the dissolution kettle, filtering separation filtrate and filter residue, filter residue is washed through diluted acid, washed with water again till the neutrality, filter, drying is packed to such an extent that specific surface area is 690m
2/ g, iodine sorption value are the activated carbon product of 2068mg/g.
Embodiment 2: the ratio uniform mixing that with rice hull ash, solid sodium carbonate in mass ratio is 1: 1.75, place High Temperature Furnaces Heating Apparatus to be warming up to 875 ℃, the constant temperature frit reaction stops heating after 1 hour, be cooled in 100 ℃, is transferred to and is heated to boiling dissolving 1 hour in the dissolution kettle, filtering separation filtrate and filter residue, filter residue is washed through diluted acid, washed with water again till the neutrality, filter, drying is packed to such an extent that specific surface area is 355m
2/ g, iodine sorption value are the activated carbon product of 1063mg/g.
Embodiment 3: the ratio uniform mixing that with rice hull ash, solid sodium carbonate in mass ratio is 1: 1.75, place High Temperature Furnaces Heating Apparatus to be warming up to 900 ℃, stop heating behind the constant temperature frit reaction 1h, be cooled in 100 ℃, be transferred to and be heated to boiling dissolving 1h in the dissolution kettle, filtering separation filtrate and filter residue, filter residue is washed through diluted acid, washes with water till the neutrality again, filters, drying is packed to such an extent that specific surface area is 380m
2/ g, iodine sorption value are the activated carbon product of 1138mg/g.
Embodiment 4: the ratio uniform mixing that with rice hull ash, solid sodium carbonate in mass ratio is 1: 1.75, place High Temperature Furnaces Heating Apparatus to be warming up to 900 ℃, stop heating behind the constant temperature frit reaction 45min, be cooled in 100 ℃, be transferred to and be heated to boiling dissolving 1h in the dissolution kettle, filtering separation filtrate and filter residue, filter residue is washed through diluted acid, washes with water till the neutrality again, filters, drying is packed to such an extent that specific surface area is 460m
2/ g, iodine sorption value are the activated carbon product of 1378mg/g.
Embodiment 5: the ratio uniform mixing that with rice hull ash, solid sodium carbonate in mass ratio is 1: 2, place High Temperature Furnaces Heating Apparatus to be warming up to 900 ℃, stop heating behind the constant temperature frit reaction 45min, be cooled in 100 ℃, be transferred to and be heated to boiling dissolving 1h in the dissolution kettle, filtering separation filtrate and filter residue, filter residue is washed through diluted acid, washed with water again till the neutrality, filter, drying is packed to such an extent that specific surface area is 385m
2/ g, iodine sorption value are the activated carbon product of 1154mg/g.
Embodiment 6: the ratio uniform mixing that with rice hull ash, solid sodium carbonate in mass ratio is 1: 1.75, place High Temperature Furnaces Heating Apparatus to be warming up to 900 ℃, stop heating behind the constant temperature frit reaction 45min, be cooled in 100 ℃, be transferred to and be heated to boiling dissolving 1.5h in the dissolution kettle, filtering separation filtrate and filter residue, filter residue is washed through diluted acid, washed with water again till the neutrality, filter, drying is packed to such an extent that specific surface area is 500m
2/ g, iodine sorption value are the activated carbon product of 1498mg/g.
Embodiment 7: the filtrate that step (1) is obtained places reactor, adjusting temperature is 80 ℃, feeding contains 30wt% carbon dioxide mix gas carbon reaction 1h, ageing 3h, filter, filter cake washing, drying, crushing packing get that particle diameter is that 39nm, purity are 99.2%, whiteness is 99.3% silica product.
Embodiment 8: the filtrate that step (1) is obtained places reactor, adjusting temperature is 90 ℃, feed 30wt% carbon dioxide mix gas carbon reaction 1h, ageing 3h, filter, filter cake washing, drying, crushing packing get that median size is that 41nm, purity are 99.3%, whiteness is 99.5% silica product.
Claims (3)
1. one kind is utilized rice hull ash to prepare silicon-dioxide and process of active carbon, and concrete steps are as follows:
(1) high-temperature fusion activation, filter residue prepares gac
Is 1: 1.5～3.0 ratio uniform mixing with rice hull ash, solid sodium carbonate or salt of wormwood in mass ratio, places High Temperature Furnaces Heating Apparatus to be warming up to 850～950 ℃, the constant temperature frit reaction, reclaim tail gas simultaneously, react and stop heating after 0.5～2 hour, be cooled in 100 ℃, be transferred to and be heated to boiling dissolving in the dissolution kettle 0.5～2 hour, filtering separation filtrate and filter residue, filter residue is washed through diluted acid, washed with water again till the neutrality, filter, drying, pack activated carbon product.
(2) filtrate prepares silicon-dioxide
The filtrate of step (1) is placed reactor, and adjusting temperature is 70～95 ℃, feeds mixed tail gas in (1), carbonization 1h, ageing 3h filters, the filtrate condensing crystal returns step (1) recycle, filter cake washing, drying, pulverizing, pack silica product.
2. the method for claim 1, it is characterized in that: rice hull ash and yellow soda ash or salt of wormwood heating and melting discharge carbonic acid gas, merge with the rice husk combustion tail gas, adjusting the carbonic acid gas massfraction is 25～40%, is used for step (2) carburizing reagent, recycle.
3. the method for claim 1 is characterized in that: filtrate in the step (2), reclaim yellow soda ash or salt of wormwood through condensing crystal, and return step (1) recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010162142XA CN101804988B (en) | 2010-05-05 | 2010-05-05 | Novel method for preparing silicon dioxide and active carbon from rice hull ash |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010162142XA CN101804988B (en) | 2010-05-05 | 2010-05-05 | Novel method for preparing silicon dioxide and active carbon from rice hull ash |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101804988A CN101804988A (en) | 2010-08-18 |
| CN101804988B true CN101804988B (en) | 2011-12-14 |
Family
ID=42606971
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010162142XA Expired - Fee Related CN101804988B (en) | 2010-05-05 | 2010-05-05 | Novel method for preparing silicon dioxide and active carbon from rice hull ash |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101804988B (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190509A (en) * | 2011-03-16 | 2011-09-21 | 吉林大学 | Method for producing silicon fertilizer from rice straws |
| CN103508459A (en) * | 2012-06-26 | 2014-01-15 | 王金山 | Technology for producing white carbon black and active carbon from rice hull |
| CN102923702A (en) * | 2012-10-10 | 2013-02-13 | 上海大学 | Method for preparing active carbon from waste printed circuit board |
| CN103332994B (en) * | 2013-07-25 | 2015-07-22 | 王兢 | Method and system for comprehensively utilizing biomass ash |
| CN104071789A (en) * | 2014-07-14 | 2014-10-01 | 武汉大学 | Method for preparing capacitive active carbon powder through biomaterial treated by fused salt |
| CN104150478B (en) * | 2014-07-17 | 2016-06-15 | 吉林大学 | A kind of green circulatory technique of being prepared activated carbon for super capacitors material by rice husk |
| CN104163427B (en) * | 2014-07-21 | 2018-01-16 | 大连理工大学 | A kind of method that activated carbon is prepared using fuse salt activation |
| CN104258889A (en) * | 2014-09-17 | 2015-01-07 | 南京理工大学 | Method utilizing K-based pyrolysis catalyst |
| CN106540696A (en) * | 2016-11-14 | 2017-03-29 | 天津工业大学 | A kind of method prepared by rice husk base metal supported catalyst mesoporous silicon oxide |
| CN107188170A (en) * | 2017-06-01 | 2017-09-22 | 镇江四联机电科技有限公司 | A kind of use mixed base activation prepares the production technology of activated carbon |
| CN113173585B (en) * | 2020-06-09 | 2023-02-07 | 长春瑛隆材料科技有限公司 | Method for preparing high-quality silicon dioxide from carbonized rice hulls |
| CN112194146A (en) * | 2020-09-24 | 2021-01-08 | 长春工业大学 | Preparation method of biomass-based nano silicon dioxide with high specific surface area |
| CN114634184B (en) * | 2020-12-16 | 2023-07-14 | 安徽进化硅纳米材料科技有限公司 | Utilization method of biomass |
| CN113998887B (en) * | 2021-11-26 | 2022-09-09 | 常州隆兴玻璃制品厂 | High borosilicate glass tube with chemical stability and processing technology thereof |
| CN114479179B (en) * | 2022-03-02 | 2022-10-18 | 吉林大学 | Nitrogen-doped nano silicon dioxide/carbon black hybrid material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057065C (en) * | 1998-06-12 | 2000-10-04 | 吉林大学 | Preparation of superhigh specific surface area active carbon |
| CN101417798B (en) * | 2008-11-26 | 2011-05-11 | 吉林大学 | Paddy hull burned gas and waste residue comprehensive utilization method |
-
2010
- 2010-05-05 CN CN201010162142XA patent/CN101804988B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101804988A (en) | 2010-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101804988B (en) | Novel method for preparing silicon dioxide and active carbon from rice hull ash | |
| CN101417798B (en) | Paddy hull burned gas and waste residue comprehensive utilization method | |
| CN100391841C (en) | Method for industrial production of white carbon black using rice husk | |
| CN102515279B (en) | Comprehensive extraction method of ferro-silico-aluminum in gangue | |
| CN101993087A (en) | Method for preparing water glass by using fly ash | |
| CN102219257B (en) | Method for preparing vanadium pentoxide | |
| CN102627305B (en) | Method using alkaline process to extract alumina in coal ash | |
| CN104402017B (en) | A kind of method of synthetic zeolite from flyash | |
| CN1903725A (en) | Comprehensive utilization treatment tachnology of aluminium waste slag, waste ash | |
| CN103693650A (en) | Method for producing nano silicon dioxide and nano calcium carbonate by using rice hull ash and flue gas of biomass power plant | |
| CN101704526B (en) | Method for producing white carbon black and active carbon by using residual rice hull ash after gasification | |
| CN104773744B (en) | A kind of by old stew in soy sauce for high-purity magnesium oxide method | |
| CN102220478A (en) | Preparation method for vanadium pentoxide | |
| NO150954B (en) | PROCEDURE FOR THE PREPARATION OF SILICON Dioxide-SUSTAINED WASTE FLUID TO EXCIPIENTIC SILICIDE OR SILICATE | |
| CN114180604A (en) | Comprehensive utilization method of waste residues in spice production and synthetic ammonia purge gas | |
| CN102675082B (en) | Preparation method of calcium propionate by egg shell | |
| CN108658092B (en) | Method for preparing P-type molecular sieve and high-silicon mordenite from aluminum residue extracted by fly ash acid method and utilization method of fly ash | |
| CN106044784B (en) | A kind of method using flyash production high-purity silicon dioxide | |
| CN103663505A (en) | Method for treating potassium feldspar according to sub-molten salt method to prepare potassium carbonate | |
| CN105502426A (en) | Method for preparing water glass through extracting silicon oxide from chrysotile tailings by strong-base roasting method | |
| CN101633584B (en) | A method for producing nitrogen phosphorus potassium compound fertilizer with water-insoluble potassium-containing rock | |
| CN104743565A (en) | Method for preparing zeolite molecular sieve through coal ash | |
| CN101374767B (en) | An improved process for preparation of magnesium oxide | |
| CN102500184A (en) | Closed-circuit recycling process of waste gas and waste residue generated during production of brown fused alumina and calcium carbide | |
| CN103601210A (en) | Method for synthesizing zeolite by one-step alkali dissolution of bentonite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| 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: 20111214 Termination date: 20210505 |