CN101691225B - Method for coproducing nano silicon dioxide and active carbon from rice hull ash - Google Patents
Method for coproducing nano silicon dioxide and active carbon from rice hull ash Download PDFInfo
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- CN101691225B CN101691225B CN2009102723521A CN200910272352A CN101691225B CN 101691225 B CN101691225 B CN 101691225B CN 2009102723521 A CN2009102723521 A CN 2009102723521A CN 200910272352 A CN200910272352 A CN 200910272352A CN 101691225 B CN101691225 B CN 101691225B
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Abstract
The invention relates to a method for coproducing nano silicon dioxide and active carbon by using rice hull ash as a raw material. The method comprises the following steps: (1) adding alkali liquor into the rice hull ash to perform reaction, and filtering a reaction product after the reaction is finished to obtain filter liquor and carbon filter residue; (2) adding the alkali liquor into the filter liquor; (3) adding ethyl acetate into the filter liquor to perform reaction, and standing the solution to form gel; (4) acidifying the solution, and drying an acidified product to obtain the nano silicon dioxide; (5) adding diluted hydrochloric acid solution into the carbon filter residue to perform pretreatment, and then washing the solution to be neutral; (6) then adopting the alkali liquor as an activating agent to perform activation, and soaking the activated carbon filter residue into hydrochloric acid; and (7) drying the carbon filter residue washed to be neutral to obtain the active carbon. The method has the advantage of simple process, the nano silicon dioxide and the active carbon prepared by the method have excellent performance, and the value of the rice hull ash realizes maximum benefit.
Description
Technical field
The present invention relates to a kind of process method for preparing nano silicon, specifically a kind of is raw material with the rice hull ash, and the coproduction of applied acetic acid ethyl ester sol-gel method prepares nano silicon and process of active carbon.
Background technology
Paddy rice is about 200,000,000 tons of the annual ultimate production of China, and rice husk is a sub product main in the paddy course of processing, accounts for 18%～20% of paddy by weight.About 4,000 ten thousand tons of the annual rice husk that produces of China.These rice husks are used to burning or generating more, obtain the residue rice hull ash and are about 20% of rice husk.Present stage is few to the development and use research of discarded rice hull ash; The rice hull ash that obtains is taken as offal treatment more, because the little stacking volume of rice hull ash density is big, contains a large amount of silicon and is difficult for degraded; What cause rice hull ash deposits and is treated as a difficult problem, has caused the burden of enterprise and the pollution of environment.
Staple in the rice hull ash all is SiO
2, in the rice hull ash of perfect combustion, 95.5%SiO is arranged
2, and 60% SiO is nearly also arranged in unburnt
2Research shows that rice husk is through the non-crystalline state SiO of biomineralization mode enrichment
2Form with nano particle exists.Other there are some researches show the SiO in the rice hull ash that is obtained by the rice husk burning
2It is amorphous state.Amorphous state SiO
2Have bigger reactive behavior, be soluble in alkali lye and make the various types of silicon Barbiturates, and can further make nanoscale SiO by silicate
2
Nanometer SiO
2Unusual characteristics such as high-strength, the high-ductility that still has under the quantum size that has, quantum tunneling effect and its special light, electrical characteristic, high magnetic resistance phenomenon, thyrite phenomenon and the high temperature, good stability make nanometer SiO
2Can be widely used in electronic package material, polymer composite, plastics, coating, rubber, pigment, pottery, tackiness agent, glass reinforced plastic, pharmaceutical carrier, makeup and kill field such as mattress material.
And do not contain the heavy metals that are harmful to health such as arsenic, lead in the rice hull ash, get rid of pollutions such as agricultural chemicals through burning again.Can make high-quality silicate by rice hull ash, this silicate is to make high quality nano SiO
2Good raw material.In addition, for the carbon that exists nearly 40% in the unburnt rice hull ash, these carbon can be in order to the preparation gac.
In recent years because gac is inhaled, desorption rate is fast, advantage such as can reuse, every field such as it is refining in environmental protection, chemical industry, food-processing, hydrometallurgy, medicine, military chemistry protection are used widely.Gac has become a big focus in raw material of wood-charcoal material field.The preparation of gac also receives publicity day by day; The main raw material of early stage preparation gac is Forest products such as timber, sawdust, shell; But this type of resource of China is very limited, and is difficult for concentrating, storing, and therefore changes raw material structure; Effectively utilizing waste and produce gac, is the inexorable trend of China's gac industry development.Utilize rice hull ash to prepare SiO
2Obtain useless filter residue and prepare gac, not only more fully effectively utilized rice hull ash, and can be used as the substitute of precious resources such as timber, economize on resources.
Rice husk is a renewable resources, and the rice hull ash of utilizing its burning to make prepares the nanometer SiO of high added value
2And gac, prepare SiO compared with original process using ore
2With activation prepares gac as raw material with Forest products, more reasonable and persistent utilization material and resource, can satisfy more that current recycling economy advocates with the harmonious Economic Development Mode of environment.
More existing preparation technologies, adopt rice husk is raw material more, each goods of burning back preparation under the temperature control condition, and how rice husk has been used for combustion heat supplying by enterprise owing to have the high combustion value, its temperature of combustion can not be controlled.And rice husk is bulky, is difficult for storing and transportation.Utilize the depleted rice hull ash after enterprise burns to prepare SiO
2And gac, can effectively utilize rice hull ash, not only can solve the rice hull ash pollution problem, improve the comprehensive deep development utilization of rice husk, can also make be widely used, high value-added product, improved the added value that paddy is produced greatly.Get agricultural profit to promoting, improve farmers' income, have bigger social effect and more practical value.
Summary of the invention
The object of the invention is exactly the defective to prior art, provides a kind of rice hull ash coproduction to prepare nano silicon and process of active carbon.
Technical scheme of the present invention is achieved in that it may further comprise the steps:
(1), adding alkali lye reacts in rice hull ash, after having reacted reaction product is filtered, and obtains filtrating and charcoal filter residue;
(2), in filtrating, add alkali lye, adjustment silicate modulus to 1.5～2.5; Modulus is the mol ratio of silicon-dioxide and alkalimetal oxide in the silicate solutions.
(3), again add ETHYLE ACETATE and react, static one-tenth glue;
(4), dripping dilute acid is carried out acidifying again, regulate about pH to 4, spinning, washing be to detecting in the supernatant not chloride ion-containing with silver nitrate solution, separates, obtains nano silicon after the drying;
(5), in the charcoal filter residue, add the concussion of 10% dilute hydrochloric acid solution, suction filtration, washing is to neutral then; Every gram charcoal filter residue adds 10～15ml hydrochloric acid soln;
(6), then adopt alkali lye to carry out activation as acvator, the charcoal filter residue after the activation is used the salt soak, and washing is to neutral then;
(7), will wash to neutral charcoal filter residue oven dry, obtain gac.
When wherein adding alkali lye reacted in rice hull ash, the alkali of adding and the mass ratio of rice hull ash were 2: 10～4: 10, and temperature of reaction is 120～160 ℃, and the reaction times is 5～7 hours; Wherein said alkali lye is sodium hydroxide or potassium hydroxide solution; When adding ETHYLE ACETATE reacted, temperature of reaction was 40～55 ℃, and the reaction times is 35～45 minutes, to the jelly shape gel that forms micro emulsion white; The concentration of ETHYLE ACETATE is 0.7～0.9mol/L, and the add-on of ETHYLE ACETATE is 1.6～1.8: 1 for the volume ratio with silicate; The activation of charcoal filter residue adopts KOH as acvator, and mass percent concentration is 23～27%, and every gram charcoal filter residue is with 18～22mlKOH solution; Flood after 12 hours, filter supernatant, 120～140 ℃ of bakings are to half-dried postactivated; Activation temperature is 600～750 ℃, and soak time is 18～30 minutes; Every gram filter residue use 5～10ml mass percent after the activation is 15% salt soak, washing while stirring, and washing is to neutral then.
The nano silicon that the present invention adopts the ETHYLE ACETATE sol-gel method to prepare, its particle diameter reach nanometer SiO at 40～90nm
2Granularity requirements.Full spectrum direct-reading inductively coupled plasma Atomic Emission SpectrometerAES belongs to qualitative and quantitative analysis to impurity unit and can know that total impurities content is 0.147% in this product, is high-purity Si O
2The infrared absorption spectrum characterization result shows that this product is amorphous state nanometer SiO
2
The gac methylene radical adsorptive power of KOH after as Treatment with activating agent is 14.6ml/0.1g, satisfies the 12.0ml/0.1g of national standard, is superior to the 12.8ml/0.1g of commercially available gac.
The depleted rice hull ash of the present invention after with industrial combustion is raw material, preparation nano level SiO
2With the gac of high adsorptive power, it has advantage of simple technology, the nano silicon of the present invention preparation and Properties of Activated Carbon excellence, make rice hull ash Value Realization greatest benefitization.
Description of drawings
Fig. 1 is a schema of the present invention
Embodiment
Below in conjunction with embodiment the present invention is done and to further describe:
Embodiment 1:
The present invention includes following steps:
(1), adding alkali lye reacts in rice hull ash, after having reacted reaction product is filtered, and obtains filtrating and charcoal filter residue;
(2), in filtrating, add alkali lye, adjustment silicate modulus to 1.5～2.5; Modulus is the mol ratio of silicon-dioxide and alkalimetal oxide in the silicate solutions.
(3), again add ETHYLE ACETATE and react, static one-tenth glue;
(4), dripping dilute acid is carried out acidifying again, regulate about pH to 4, spinning, washing be to detecting in the supernatant not chloride ion-containing with silver nitrate solution, separates, obtains nano silicon after the drying;
(5), in the charcoal filter residue, add the concussion of 10% dilute hydrochloric acid solution, suction filtration, washing is to neutral then; Every gram charcoal filter residue adds 10～15ml hydrochloric acid soln;
(6), then adopt alkali lye to carry out activation as acvator, the charcoal filter residue after the activation is used the salt soak, and washing is to neutral then;
(7), will wash to neutral charcoal filter residue oven dry, obtain gac.
When wherein adding alkali lye reacted in rice hull ash, the alkali of adding and the mass ratio of rice hull ash were 2: 10, and temperature of reaction is 120 ℃, and the reaction times is 5 hours; Wherein said alkali lye is potassium hydroxide solution; When adding ETHYLE ACETATE reacted, temperature of reaction was 40～55 ℃, and the reaction times is 35～45 minutes, to the jelly shape gel that forms micro emulsion white; The concentration of ETHYLE ACETATE is 0.7mol/L, and the add-on of ETHYLE ACETATE is 1.6: 1 for the volume ratio with silicate; The activation of charcoal filter residue adopts KOH as acvator, and mass percent concentration is 23%, and every gram charcoal filter residue is used 18mlKOH solution, floods after 12 hours, filters supernatant, and 120 ℃ of bakings are to half-dried postactivated, and activation temperature is 600 ℃, and soak time is 20 minutes; Every gram charcoal filter residue use 5ml mass percent after the activation is 15% salt soak, washing while stirring, and washing is to neutral then.
Embodiment 2:
The present invention includes following steps:
(1), adding alkali lye reacts in rice hull ash, after having reacted reaction product is filtered, and obtains filtrating and charcoal filter residue;
(2), in filtrating, add alkali lye, adjustment silicate modulus to 1.5～2.5; Modulus is the mol ratio of silicon-dioxide and alkalimetal oxide in the silicate solutions.
(3), again add ETHYLE ACETATE and react, static one-tenth glue;
(4), dripping dilute acid is carried out acidifying again, regulate about pH to 4, spinning, washing be to detecting in the supernatant not chloride ion-containing with silver nitrate solution, separates, obtains nano silicon after the drying;
(5), in the charcoal filter residue, add the concussion of 10% dilute hydrochloric acid solution, suction filtration, washing is to neutral then; Every gram charcoal filter residue adds 10～15ml hydrochloric acid soln;
(6), then adopt alkali lye to carry out activation as acvator, the charcoal filter residue after the activation is used the salt soak, and washing is to neutral then;
(7), will wash to neutral charcoal filter residue oven dry, obtain gac.
When wherein adding alkali lye reacted in rice hull ash, the alkali of adding and the mass ratio of rice hull ash were 4: 10, and temperature of reaction is 160 ℃, and the reaction times is 7 hours; Wherein said alkali lye is sodium hydroxide solution; When adding ETHYLE ACETATE reacted, temperature of reaction was 40～55 ℃, and the reaction times is 35～45 minutes, to the jelly shape gel that forms micro emulsion white; The concentration of ETHYLE ACETATE is 0.9mol/L, and the add-on of ETHYLE ACETATE is 1.8: 1 for the volume ratio with silicate; The activation of charcoal filter residue adopts KOH as acvator, and mass percent concentration is 27%, and every gram charcoal filter residue is used 22mlKOH solution, floods after 12 hours, filters supernatant, and 140 ℃ of bakings are to half-dried postactivated, and activation temperature is 750 ℃, and soak time is 18～30 minutes; Every gram filter residue use 5～10ml mass percent after the activation is 15% salt soak, washing while stirring, and washing is to neutral then.
Embodiment 3:
The preparation method is with embodiment 1.When wherein adding alkali lye reacted in rice hull ash, the alkali of adding and the mass ratio of rice hull ash were 3: 10, and temperature of reaction is 150 ℃, and the reaction times is 6 hours; Wherein said alkali lye is potassium hydroxide solution; When adding ETHYLE ACETATE reacted, temperature of reaction was 40～55 ℃, and the reaction times is 35～45 minutes, to the jelly shape gel that forms micro emulsion white; The concentration of ETHYLE ACETATE is 0.8mol/L, and the add-on of ETHYLE ACETATE is 1.7: 1 for the volume ratio with silicate; The activation of charcoal filter residue adopts sodium hydroxide as acvator, and mass percent concentration is 23～27%, and every gram charcoal filter residue is used the 20ml sodium hydroxide solution; Flood after 12 hours, filter supernatant, 140 ℃ of bakings are to half-dried postactivated; Activation temperature is 625 ℃, and soak time is 18～30 minutes; Every gram filter residue use 5～10ml mass percent after the activation is 15% salt soak, washing while stirring, and washing is to neutral then.
Claims (1)
1. a rice hull ash coproduction prepares nano silicon and process of active carbon, and it may further comprise the steps:
(1), adding alkali lye reacts in rice hull ash, after having reacted reaction product is filtered, and obtains filtrating and charcoal filter residue;
(2), in filtrating, add alkali lye, adjustment silicate modulus to 1.5～2.5; Modulus is the mol ratio of silicon-dioxide and alkalimetal oxide in the silicate solutions;
(3), again add ETHYLE ACETATE and react, static one-tenth glue;
(4), dripping dilute acid is carried out acidifying again, regulate pH to 4, spinning, washing be to detecting in the supernatant not chloride ion-containing with silver nitrate solution, separates, obtains nano silicon after the drying;
(5), in the charcoal filter residue, add the concussion of 10% dilute hydrochloric acid solution, suction filtration, washing is to neutral then; Every gram charcoal filter residue adds 10～15mL hydrochloric acid soln;
(6), then adopt alkali lye to carry out activation as acvator, the charcoal filter residue after the activation is used the salt soak, and washing is to neutral then;
(7), will wash to neutral charcoal filter residue oven dry, obtain gac;
When wherein adding alkali lye reacted in rice hull ash, the alkali of adding and the mass ratio of rice hull ash were 2: 10, and temperature of reaction is 120 ℃, and the reaction times is 5 hours; Wherein said alkali lye is potassium hydroxide solution; When adding ETHYLE ACETATE reacted, temperature of reaction was 40～55 ℃, and the reaction times is 35～45 minutes, to the jelly shape gel that forms micro emulsion white; The concentration of ETHYLE ACETATE is 0.7mol/L, and the add-on of ETHYLE ACETATE is 1.6: 1 for the volume ratio with silicate; The activation of charcoal filter residue adopts KOH as acvator, and mass percent concentration is 23%, and every gram charcoal filter residue is used 18mLKOH solution, floods after 12 hours, filters supernatant, and 120 ℃ of bakings are to half-dried postactivated, and activation temperature is 600 ℃, and soak time is 20 minutes; Every gram charcoal filter residue use 5mL mass percent after the activation is 15% salt soak, washing while stirring, and washing is to neutral then.
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| CN2009102723521A CN101691225B (en) | 2009-09-29 | 2009-09-29 | Method for coproducing nano silicon dioxide and active carbon from rice hull ash |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101837948B (en) * | 2010-05-05 | 2013-01-09 | 吉林大学 | Novel method of rice hull liquification and integrated utilization |
| CN101920966B (en) * | 2010-07-21 | 2012-07-04 | 化工部长沙设计研究院 | Method for producing porous nano silica and active carbon by utilizing rice hull ash |
| CN102389774B (en) * | 2011-09-28 | 2013-12-18 | 常州大学 | Method for preparing oil gas absorbing composite material |
| CN103332994B (en) * | 2013-07-25 | 2015-07-22 | 王兢 | Method and system for comprehensively utilizing biomass ash |
| CN103496697B (en) * | 2013-09-30 | 2015-10-07 | 四川大学 | A kind of method being prepared gac by rice husk thermal decomposition charcoal |
| CN104310410A (en) * | 2014-10-14 | 2015-01-28 | 叶阳 | Combined carbonization method for preparing baking soda and white carbon black by matching rice hull power generation |
| CN109175351B (en) * | 2018-10-31 | 2020-07-10 | 南京林业大学 | Method for preparing powder metallurgy friction material by adopting bio-based amorphous silicon dioxide |
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| CN101264885A (en) * | 2008-04-10 | 2008-09-17 | 江南大学 | Method for preparing high grade activated carbon from rice husk ash |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101264885A (en) * | 2008-04-10 | 2008-09-17 | 江南大学 | Method for preparing high grade activated carbon from rice husk ash |
Non-Patent Citations (3)
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