CN101402458A - Method for producing nano-scale white carbon black with rice hull ash - Google Patents
Method for producing nano-scale white carbon black with rice hull ash Download PDFInfo
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- CN101402458A CN101402458A CNA2008101070699A CN200810107069A CN101402458A CN 101402458 A CN101402458 A CN 101402458A CN A2008101070699 A CNA2008101070699 A CN A2008101070699A CN 200810107069 A CN200810107069 A CN 200810107069A CN 101402458 A CN101402458 A CN 101402458A
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Abstract
The invention relates to a method for preparing nanometer level white carbon black by rice husk ash. The method is characterized in that the process method comprises the following steps: the rice husk ash is treated by an alkaline method to prepare soluble glass; and a soluble glass solution is subjected to condensation, heat insulation, acidic reaction, aging, rinsing, filtering, preparing, homogenizing, spraying and drying, and airflow pulverization. The method has the technical effects that the method reduces cost, improves corrosion resistance, high hardness and high toughness of the material, and has simple preparation process flow, low production cost and good stability.
Description
Technical field
The present invention relates to a kind of method for preparing nano-scale white carbon black, relate in particular to a kind of method with producing nano-scale white carbon black with rice hull ash.
Background technology
Mainly be to be the raw material production white carbon black with inorganic mineral resources such as sulfuric acid alkylation acid sludges both at home and abroad, rarely having with the rice husk is raw material production white carbon black report, and the research that has some rice husks to produce white carbon black is being actively developed.
The resource of China's rice husk is extremely abundant, and at present mostly as primary fuel, and the rice hull ash after the burning mostly further do not handle, not only combine and to close utilization ratio very low, and the contaminated solution problem of failing.
China is the world main paddy producing country, and rice husk accounts for the 18%-22% of paddy kernel weight as the byproduct after the paddy processing.Contain 15~20% amorphous hydrated silica in the rice husk, other composition is mainly hydrocarbon polymer.Siliceous higher in the rice husk, the content that adopts silicon-dioxide in the available rice hull ash of incomplete combustion pyrolysis rice husk about 50%~60%, carbon about 35%~40%.All the other still have the oxide compound of micro-Ca, Mg, K, P, Fe.The tradition rice husk is mostly as the primary fuel utilization, and the rice hull ash after the burning is not mostly handled, and is little because of its density, volume is big, and environment has been caused pollution.Rice husk is after perfect combustion, and its ash content contains SiO
2About about 95%, can be used as the raw material of producing white carbon black and nano-scale white carbon black, rice husk incomplete combustion part, its structure are the hollow reticulated structure of C, are the desirable feedstock of producing gac.Nano carbon white has particle diameter little (less than 100nm), specific surface area is big (generally greater than 100m
2/ g), feature such as chemical purity height, dispersing property be good, with its superior stability, reinforcement, thickening property and thixotropy, compare the effect of common white carbon black nano-scale white carbon black and be not only reinforcement, it also has many new performances, this mainly is to utilize Nano carbon white printing opacity, granularity little, be used widely at many industrial circles such as rubber, coating, medicine, papermaking, and provide novel material basis and technical guarantee for the development in its related industries field.
Summary of the invention
The object of the present invention is to provide a kind of method with producing nano-scale white carbon black with rice hull ash, this method is raw material with the rice hull ash, adopt chemical precipitation method to prepare nano-scale white carbon black, this method has not only reduced cost greatly, and the nano-scale white carbon black quality of producing is near the nano-scale white carbon black of being produced by vapor phase process.
The present invention is achieved like this, and it is characterized in that the processing method step is:
1, the alkaline process Processing of Preparation water glass of rice hull ash: take by weighing the certain mass rice hull ash, place reactor.Pour a certain amount of NaOH solution that boils into.After reaction finishes, filter immediately, and with a certain amount of deionized water wash that boils.Reclaim filtrate, filter residue is washed with water to neutrality, puts into baking oven dry 12h under 105 ℃.
2, concentrating of water glass solution: the water glass solution of making is concentrated to 13-15 ° of Be.
3, insulation: get a certain amount of rare water glass solution with graduated cylinder, pour in the storage tank, constant temperature (30 ℃) is insulation 24h down.
4, acid-respons: a certain amount of water glass solution is added paucidisperse agent and tensio-active agent in having the reactor of stirring rake, fully dissolving back temperature control is 62 ± 2 ℃, the control rotating speed of agitator, strict control vitriolic rate of addition, timing sampling is measured the pH of material, reach till 6 until the pH of solution value, stop to add acid this moment, continue isothermal reaction to 62min.
5, ageing: with 95 ℃ of reacted solid-liquid mixture temperature controls and stirring, slaking 1.5h.
6, rinsing, filtration: the above-mentioned solution that obtains is separated with whizzer, use distilled water repetitive scrubbing 5 times, in filtrate, do not have Cl
-Till.
7, allotment: adjust with sulfuric acid about the pH to 3 of solution.
8, homogeneous: the worry cake after will allocating adds an amount of distilled water diluting, is adjusted into 40Mpa pressure with clarifixator and carries out homogeneous.
9, spraying drying: regulating inlet temperature is 240-250 ℃, and air outlet temperature is 100-105 ℃ material carried out spraying drying.
10, comminution by gas stream: the product after the spraying drying is carried out comminution by gas stream.
Technique effect of the present invention is: reduced cost, improved corrosion-resistant, high hard, the high-ductility of its material, preparation technology's flow process is simple, and low production cost has satisfactory stability.
Embodiment
Embodiment is:
The rice hull ash 40g that takes by weighing through micronizing places round-bottomed flask, then by 2: 5 (solid masses: liquid volume) of solid-to-liquid ratio, pour the NaOH solution that the 100ml concentration of boiling is 2mol/l into, load onto condensation reflux unit on round-bottomed flask, place boiling water bath to react 4h round-bottomed flask, question response finishes to use immediately the filter flask suction filtration, wash twice with the deionization poach that 200ml boils, reclaim merging filtrate, filter residue is washed with water to neutrality, puts 105 ℃ of oven dry of baking oven 12h.
Above-mentioned water glass solution is concentrated to 14 ° of Be with Rotary Evaporators, 14 ° of Be of measuring 200ml pour in the 250ml beaker, be positioned in the thermostat container, be incubated 24h down at 30 ℃, under the magnetic stirring apparatus effect, add small amount of sodium chloride (11.7g), add polyethylene glycol 6000, fully dissolving back temperature control is 62 ± 2 ℃, 80r/min, the sulfuric acid that adds 0.6mol/l with separating funnel, the control rate of addition is 0.02-0.08mL/gmin, and timing sampling is measured the pH of material, reaches till 6 until the pH of solution value.Stop to add acid this moment, continue isothermal reaction to 62min, 95 ℃ of temperature controls also stir, and slaking 1.5h separates the above-mentioned solution that obtains with whizzer, with distilled water washing repeatedly 5 times, do not have cL in filtrate
-Till, the worry cake after the washing is placed sesame seed cake and titration sulfuric acid again, adjust about the pH to 3 of solution.Adjusted worry cake is added distilled water diluting to 1400ml, be adjusted into 40Mpa pressure with clarifixator and carry out homogeneous, regulating inlet temperature is 250-260 ℃, and air outlet temperature is 100-105 ℃ to carry out spraying drying to material and can obtain nano-scale white carbon black about 70nm.
Claims (1)
1, a kind of method with producing nano-scale white carbon black with rice hull ash is characterized in that the processing method step is:
(1) the alkaline process Processing of Preparation water glass of rice hull ash: take by weighing the certain mass rice hull ash, place reactor, pour a certain amount of NaOH solution that boils into, after reaction finishes, filter immediately, and, reclaim filtrate with a certain amount of deionized water wash that boils, filter residue is washed with water to neutrality, puts into baking oven dry 12h under 105 ℃;
(2) concentrating of water glass solution: the water glass solution of making is concentrated to 13-15 ° of Be;
(3) insulation: get a certain amount of rare water glass solution with graduated cylinder, pour in the storage tank, constant temperature is incubated 24h down at 30 ℃;
(4) acid-respons: a certain amount of water glass solution is added paucidisperse agent and tensio-active agent in having the reactor of stirring rake, fully dissolving back temperature control is 62 ± 2 ℃, the control rotating speed of agitator, strict control vitriolic rate of addition, timing sampling is measured the pH of material, reach till 6 until the pH of solution value, stop to add acid this moment, continue isothermal reaction to 62min;
(5) ageing: with 95 ℃ of reacted solid-liquid mixture temperature controls and stirring, slaking 1.5h;
(6) rinsing, filtration; The above-mentioned solution that obtains is separated with whizzer, use distilled water repetitive scrubbing 5 times, in filtrate, do not have Cl
-Till;
(7) allotment: adjust with sulfuric acid about the pH to 3 of solution;
(8) homogeneous: the worry cake after will allocating adds an amount of distilled water diluting, is adjusted into 40Mpa pressure with clarifixator and carries out homogeneous;
(9) spraying drying: regulating inlet temperature is 240-250 ℃, and air outlet temperature is 100-105 ℃ material carried out spraying drying;
(10) comminution by gas stream: the product after the spraying drying is carried out comminution by gas stream.
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Cited By (14)
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CN102092721A (en) * | 2010-11-24 | 2011-06-15 | 陈君华 | Method for preparing nanoscale white carbon black through sulfuric acid precipitation method |
CN102372272A (en) * | 2011-08-15 | 2012-03-14 | 万载县辉明化工有限公司 | Preparation method of silicon dioxide for plastic film opening agent |
CN102602946A (en) * | 2012-03-21 | 2012-07-25 | 陈君华 | Method for preparing high-specific-surface white carbon black by circularly utilizing waste water including sodium sulfate |
CN103508459A (en) * | 2012-06-26 | 2014-01-15 | 王金山 | Technology for producing white carbon black and active carbon from rice hull |
CN103771425A (en) * | 2014-01-17 | 2014-05-07 | 江西恒隆实业有限公司 | Production process for preparing white carbon black by use of rice hull ash |
CN106115720A (en) * | 2016-08-14 | 2016-11-16 | 皖西学院 | A kind of method utilizing rice hull ash to prepare nano silicon |
CN106276930A (en) * | 2016-08-16 | 2017-01-04 | 海宁永欣科技咨询有限公司 | A kind of processing technology of nano-scale white carbon black |
CN106629755A (en) * | 2016-11-16 | 2017-05-10 | 浙江工业大学 | Supergravity gas-liquid precipitation method for preparing silica nanoparticles based on rice hull ash |
CN107311187A (en) * | 2017-06-28 | 2017-11-03 | 吉林化工学院 | The method that waterglass is produced with rice hull ash extract |
CN108164754A (en) * | 2017-12-28 | 2018-06-15 | 无锡恒诚硅业有限公司 | A kind of preparation method of modified white carbon black and modified white carbon black therefrom |
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CN113603422A (en) * | 2021-08-23 | 2021-11-05 | 崇德建材集团有限公司 | Anti-cracking recycled concrete |
CN113943006A (en) * | 2021-12-07 | 2022-01-18 | 安徽进化硅纳米材料科技有限公司 | High-reinforcement white carbon black and preparation method and application thereof |
CN115159529A (en) * | 2022-08-15 | 2022-10-11 | 锦洋高新材料股份有限公司 | Method for preparing white carbon black by taking industrial silicon dioxide solid waste as raw material through precipitation method |
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CN102092721A (en) * | 2010-11-24 | 2011-06-15 | 陈君华 | Method for preparing nanoscale white carbon black through sulfuric acid precipitation method |
CN102092721B (en) * | 2010-11-24 | 2012-10-31 | 陈君华 | Method for preparing nanoscale white carbon black through sulfuric acid precipitation method |
CN102372272A (en) * | 2011-08-15 | 2012-03-14 | 万载县辉明化工有限公司 | Preparation method of silicon dioxide for plastic film opening agent |
CN102602946A (en) * | 2012-03-21 | 2012-07-25 | 陈君华 | Method for preparing high-specific-surface white carbon black by circularly utilizing waste water including sodium sulfate |
CN102602946B (en) * | 2012-03-21 | 2022-04-08 | 安徽科技学院 | Method for preparing white carbon black with high specific surface area by recycling wastewater containing sodium sulfate |
CN103508459A (en) * | 2012-06-26 | 2014-01-15 | 王金山 | Technology for producing white carbon black and active carbon from rice hull |
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CN103771425B (en) * | 2014-01-17 | 2015-08-19 | 江西恒隆实业有限公司 | Rice hull ash is utilized to prepare the production technique of white carbon black |
CN106115720B (en) * | 2016-08-14 | 2017-07-14 | 皖西学院 | A kind of method that utilization rice hull ash prepares nano silicon |
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CN106276930B (en) * | 2016-08-16 | 2018-06-22 | 佛山威迪科彩色装饰涂料有限公司 | A kind of manufacture craft of nano-scale white carbon black |
CN107840340A (en) * | 2016-08-16 | 2018-03-27 | 海宁永欣科技咨询有限公司 | The manufacture craft of the nano-scale white carbon black of improvement |
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CN106276930A (en) * | 2016-08-16 | 2017-01-04 | 海宁永欣科技咨询有限公司 | A kind of processing technology of nano-scale white carbon black |
CN106629755A (en) * | 2016-11-16 | 2017-05-10 | 浙江工业大学 | Supergravity gas-liquid precipitation method for preparing silica nanoparticles based on rice hull ash |
CN107311187A (en) * | 2017-06-28 | 2017-11-03 | 吉林化工学院 | The method that waterglass is produced with rice hull ash extract |
CN108164754A (en) * | 2017-12-28 | 2018-06-15 | 无锡恒诚硅业有限公司 | A kind of preparation method of modified white carbon black and modified white carbon black therefrom |
CN108164754B (en) * | 2017-12-28 | 2020-02-21 | 无锡恒诚硅业有限公司 | Preparation method of modified white carbon black and modified white carbon black prepared by same |
CN108383128A (en) * | 2018-05-15 | 2018-08-10 | 潘荣强 | A kind of preparation method of rice husk base micro-nano structure porous silica |
CN113603422A (en) * | 2021-08-23 | 2021-11-05 | 崇德建材集团有限公司 | Anti-cracking recycled concrete |
CN113943006A (en) * | 2021-12-07 | 2022-01-18 | 安徽进化硅纳米材料科技有限公司 | High-reinforcement white carbon black and preparation method and application thereof |
CN115159529A (en) * | 2022-08-15 | 2022-10-11 | 锦洋高新材料股份有限公司 | Method for preparing white carbon black by taking industrial silicon dioxide solid waste as raw material through precipitation method |
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