CN107200334A - A kind of rice husk prepares the Efficient utilization method of white carbon - Google Patents
A kind of rice husk prepares the Efficient utilization method of white carbon Download PDFInfo
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- CN107200334A CN107200334A CN201710554604.4A CN201710554604A CN107200334A CN 107200334 A CN107200334 A CN 107200334A CN 201710554604 A CN201710554604 A CN 201710554604A CN 107200334 A CN107200334 A CN 107200334A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/155—Preparation of hydroorganogels or organogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to the preparing technical field of white carbon, the Efficient utilization method that a kind of rice husk prepares white carbon is disclosed, is comprised the following steps：（1）Rice husk is dried after over cleaning removal of impurities, pulverize, add watery hydrochloric acid and organic solvent and sodium bicarbonate solution, boiled, alkaline matter in rice husk is removed, hydrolysis of organic matter, metal ion and ethyl acetate formation metallo-organic complex, boiling the whiteness of dioxide-containing silica and white carbon after processing can be greatly enhanced（2）The mixed system cooked is cooled to 20 25 DEG C, filtered after standing 46 hours, obtained filtrate is put into acetone soln, dispersed with stirring, can put forward the hydrophobicity and compatibility of silicon compound；（3）The aerosil that mass fraction is 0.3 0.5% is added into obtained dried object, mixed calcining is carried out, obtains the high white carbon of the uniform specific surface area of particle.
Description
Technical field
The invention belongs to the preparing technical field of white carbon, and in particular to a kind of rice husk prepares the efficient utilization side of white carbon
Method.
Background technology
White carbon is the general name of white powder X-ray amorphous silicic acid and silicate product, is primarily referred to as precipitating dioxy
SiClx, aerosil and superfine silicon dioxide gel, also including powdered synthetic aluminium silicate and calcium silicates etc..White carbon is
Porous material, its composition can use SiO2·nH2O represents, wherein nH2O is present in the form of surface hydroxyl.Causticity can be dissolved in
Alkali and hydrofluoric acid, water insoluble, solvent and acid (except hydrofluoric acid).High temperature resistant, it is non-ignitable, tasteless, odorless, with it is good electricity absolutely
Edge.Be mainly used as paint filler, rubber reinforcing filler, plastics tackifier and thixotropic agent, synthetic grease silicone grease it is thick
Agent.
Element silicon on the earth's crust be ranked second, and oxygen is only second in the content of the earth's crust, and mass fraction is 26.3%.In nature,
Silicon generally exists in oxygenatedchemicals form, and feldspar, mica, clay, olivine, hornblend etc. are all silicates；Crystal,
Agate, green jade, opal, quartz, sand and flint etc. are all silicas.Silicon product is utilized using Nonmetallic Mineral Industry Exploitation, is
A kind of common mode of production.And, it is necessary to have to the activity of white carbon, purity, whiteness compatibility etc. in the production of white carbon
Higher requirement, is especially applied in high-precision field, and extraction cost height, cost are big from ore, and people start to turn sight
To plant resources, prepare white carbon using rice husk and had been reported that and patent, but it is not high to there is economic benefit, product quality
Unstable the problem of.
The content of the invention
The purpose of the present invention be for it is existing the problem of there is provided the Efficient utilization method that a kind of rice husk prepares white carbon,
By the use of rice husk as raw material, the preparation process of the intermediate product of waterglass is eliminated, production cost declines to a great extent, quality is higher than heavy
The white carbon that shallow lake method is prepared, and quality prepared by gas phase method are more or less the same.
The present invention is achieved by the following technical solutions：
A kind of rice husk prepares the Efficient utilization method of white carbon, comprises the following steps：
（1）It is 3-5% that rice husk, which is dried after over cleaning removal of impurities to water content, is pulverized, and 40-60 mesh sieves is crossed, to powdered rice hulls
It is middle addition mass fraction be 20-30% watery hydrochloric acid, mass fraction be 10-15% acetone, mass fraction be 5-8% acetic acid second
Ester and the sodium bicarbonate solution that mass fraction is 3-5%, after stirring, heating is boiled, and maintains the boiling-like of 3-4 hours
State, is during which added in heating systems using deionized water, adjusts the pH value of system between 6.8-7.0；
（2）The mixed system cooked is cooled to 20-25 DEG C, filtered after standing 4-6 hours, obtained filtrate input
Into acetone soln, it is totally submerged, the stearic acid that mass fraction is 2-3% has been dissolved in acetone soln, 55-60 DEG C has been heated to, no
Disconnected stirring is vapored away completely to acetone soln, is dried in an oven to constant weight, drying temperature is 80-90 DEG C, obtained dried object；
（3）The aerosil that mass fraction is 0.3-0.5%, 20-30 points of ultrasonic disperse are added into obtained dried object
Clock, obtained dispersion is placed in Muffle furnace and is heated to 550-650 DEG C, is calcined 3-5 hours, is obtained white particulate titanium dioxide
Pulverized after silicon, cooling, spray drying produces white carbon in 1.5-2 hours at 100-110 DEG C.
It is used as further improvement of these options, step（1）The mass concentration of middle watery hydrochloric acid is 2-3%, sodium acid carbonate
Mass concentration is 0.5-0.6%.
It is used as further improvement of these options, step（3）Described in the preparation method of aerosil be：With
Tetraethyl orthosilicate is raw material, adds the water of 2-2.5 times of volume as solvent, concentration is the hydrochloric acid of 0.15-0.20 mol/Ls
As catalyst, after mixing, it is sufficiently stirred under 280-300 revs/min, stirring liquid is put into closed insulating box at 60-65 DEG C
Lower constant temperature is placed, and is taken out after after gel generation, is placed aging 24-36 hours at room temperature, and the hydrogel after aging is utilized into super
Critical carbon dioxide method is replaced and obtains aeroge.
The present invention has advantages below compared with prior art：White carbon dust is prepared in order to solve existing rice husk and there is economy
Benefit is not high, the problem of unstable product quality, and the invention provides the Efficient utilization method that a kind of rice husk prepares white carbon, bag
Include following steps：（1）Rice husk is dried after over cleaning removal of impurities, pulverized, watery hydrochloric acid and organic solvent and carbonic acid is added
Hydrogen sodium solution, is boiled, and the alkaline matter in rice husk is removed, hydrolysis of organic matter, and metal ion forms gold with ethyl acetate
Belong to organic complex, boiling the whiteness of dioxide-containing silica and white carbon after processing can be greatly enhanced,（2）It will boil
The mixed system made is cooled to 20-25 DEG C, is filtered after standing 4-6 hours, obtained filtrate puts into acetone soln
In, dispersed with stirring can put forward the hydrophobicity and compatibility of silicon compound；（3）Mass fraction is added into obtained dried object is
0.3-0.5% aerosil, carries out mixed calcining, obtains the high white carbon of the uniform specific surface area of particle, present invention profit
With rice husk as raw material, the preparation process of the intermediate product of waterglass is eliminated, production cost declines to a great extent, quality is higher than precipitation
The white carbon that method is prepared, and quality prepared by gas phase method are more or less the same.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
A kind of rice husk prepares the Efficient utilization method of white carbon, comprises the following steps：
（1）It is 3% that rice husk, which is dried after over cleaning removal of impurities to water content, is pulverized, and crosses 40 mesh sieves, is added into powdered rice hulls
Ethyl acetate and mass fraction that acetone that watery hydrochloric acid that mass fraction is 20%, mass fraction are 10%, mass fraction are 5%
For 3% sodium bicarbonate solution, after stirring, heating is boiled, and maintains the fluidized state of 3 hours, during which uses deionized water
Add in heating systems, adjust the pH value of system between 6.8-7.0；
（2）The mixed system cooked is cooled to 20 DEG C, filtered after standing 4 hours, obtained filtrate puts into third
In ketone solution, be totally submerged, dissolved in acetone soln mass fraction be 2% stearic acid, be heated to 55 DEG C, be stirred continuously to
Acetone soln is vapored away completely, is dried in an oven to constant weight, drying temperature is 80 DEG C, obtained dried object；
（3）The aerosil that addition mass fraction is 0.3% into obtained dried object, ultrasonic disperse 20-30 minutes,
Obtained dispersion is placed in Muffle furnace and is heated to 550 DEG C, calcines 3 hours, is ground after obtaining white particulate silica, cooling
Grinds, spray drying produces white carbon in 1.5 hours at 100 DEG C.
It is used as further improvement of these options, step（1）The mass concentration of middle watery hydrochloric acid is 2%, the matter of sodium acid carbonate
It is 0.5% to measure concentration.
It is used as further improvement of these options, step（3）Described in the preparation method of aerosil be：With
Tetraethyl orthosilicate is raw material, adds the water of 2 times of volumes as solvent, concentration is used as catalysis for the hydrochloric acid of 0.15 mol/L
Agent, after mixing, is sufficiently stirred under 280 revs/min, and stirring liquid is put into closed insulating box constant temperature at 60 DEG C places, and waits to coagulate
Taken out after glue generation, place aging 24 hours at room temperature, the hydrogel after aging is replaced using supercritical carbon dioxide process
Obtain aeroge.
Embodiment 2
A kind of rice husk prepares the Efficient utilization method of white carbon, comprises the following steps：
（1）It is 4% that rice husk, which is dried after over cleaning removal of impurities to water content, is pulverized, and crosses 50 mesh sieves, is added into powdered rice hulls
Ethyl acetate and mass fraction that acetone that watery hydrochloric acid that mass fraction is 25%, mass fraction are 12%, mass fraction are 6%
For 4% sodium bicarbonate solution, after stirring, heating is boiled, and maintains the fluidized state of 3.5 hours, during which uses deionization
Water is added in heating systems, adjusts the pH value of system between 6.8-7.0；
（2）The mixed system cooked is cooled to 22 DEG C, filtered after standing 5 hours, obtained filtrate puts into third
In ketone solution, it is totally submerged, the stearic acid that mass fraction is 2.5% has been dissolved in acetone soln, 57 DEG C has been heated to, is stirred continuously
Vapor away, dry in an oven to constant weight, drying temperature is 85 DEG C, obtained dried object completely to acetone soln；
（3）The aerosil that addition mass fraction is 0.4% into obtained dried object, ultrasonic disperse 25 minutes, will
To dispersion be placed in Muffle furnace and be heated to 600 DEG C, calcine 4 hours, ground to form after obtaining white particulate silica, cooling
Powder, spray drying produces white carbon in 1.8 hours at 105 DEG C.
It is used as further improvement of these options, step（1）The mass concentration of middle watery hydrochloric acid is 2.5%, sodium acid carbonate
Mass concentration is 0.55%.
It is used as further improvement of these options, step（3）Described in the preparation method of aerosil be：With
Tetraethyl orthosilicate is raw material, adds the water of 2.3 times of volumes as solvent, concentration for 0.18 mol/L hydrochloric acid as urging
Agent, after mixing, is sufficiently stirred under 290 revs/min, and stirring liquid is put into closed insulating box constant temperature at 63 DEG C places, and treats
Taken out after gel generation, place aging 30 hours at room temperature, the hydrogel after aging is replaced using supercritical carbon dioxide process
Get aeroge in return.
Embodiment 3
A kind of rice husk prepares the Efficient utilization method of white carbon, comprises the following steps：
（1）It is 5% that rice husk, which is dried after over cleaning removal of impurities to water content, is pulverized, and crosses 60 mesh sieves, is added into powdered rice hulls
Ethyl acetate and mass fraction that acetone that watery hydrochloric acid that mass fraction is 30%, mass fraction are 15%, mass fraction are 8%
For 5% sodium bicarbonate solution, after stirring, heating is boiled, and maintains the fluidized state of 4 hours, during which uses deionized water
Add in heating systems, adjust the pH value of system between 6.8-7.0；
（2）The mixed system cooked is cooled to 25 DEG C, filtered after standing 6 hours, obtained filtrate puts into third
In ketone solution, be totally submerged, dissolved in acetone soln mass fraction be 3% stearic acid, be heated to 60 DEG C, be stirred continuously to
Acetone soln is vapored away completely, is dried in an oven to constant weight, drying temperature is 90 DEG C, obtained dried object；
（3）The aerosil that addition mass fraction is 0.5% into obtained dried object, ultrasonic disperse 30 minutes, will
To dispersion be placed in Muffle furnace and be heated to 650 DEG C, calcine 5 hours, ground to form after obtaining white particulate silica, cooling
Powder, spray drying produces white carbon in 2 hours at 110 DEG C.
It is used as further improvement of these options, step（1）The mass concentration of middle watery hydrochloric acid is 3%, the matter of sodium acid carbonate
It is 0.6% to measure concentration.
It is used as further improvement of these options, step（3）Described in the preparation method of aerosil be：With
Tetraethyl orthosilicate is raw material, adds the water of 2.5 times of volumes as solvent, concentration for 0.20 mol/L hydrochloric acid as urging
Agent, after mixing, is sufficiently stirred under 300 revs/min, and stirring liquid is put into closed insulating box constant temperature at 65 DEG C places, and treats
Taken out after gel generation, place aging 36 hours at room temperature, the hydrogel after aging is replaced using supercritical carbon dioxide process
Get aeroge in return.
Comparative example 1
With differing only in for embodiment 1, by step（1）In acetone, ethyl acetate, sodium bicarbonate solution omit, be exchanged with
The dilute hydrochloric acid solution of amount, remaining is consistent.
Comparative example 2
With differing only in for embodiment 2, by step（2）The middle mixed system cooked, is directly filtered, is dried, omitted
The process of acetone soln processing, remaining is consistent.
Comparative example 3
With differing only in for embodiment 3, by step（3）In " into obtained dried object add mass fraction be 0.5% two
The step of silica aerogel, ultrasonic disperse 30 minutes ", omits, and remaining is consistent.
Contrast test
White carbon is prepared using embodiment 1-3 and comparative example 1-3 method respectively, while being located rice hull ash in advance with existing
Reason, prepares white carbon after waterglass curing and is compared, as a control group, the product prepared to each group carries out the inspection of performance
Survey, testing result is recorded as shown in the table：
| Project | Whiteness | Dioxide-containing silica（%） | Iron content（mg/kg） | Specific surface area（m2/g） |
| Embodiment 1 | 94.7 | 99.2 | 2.36 | 235 |
| Embodiment 2 | 95.5 | 99.5 | 2.12 | 245 |
| Embodiment 3 | 95.2 | 99.3 | 2.24 | 240 |
| Comparative example 1 | 91.2 | 93.4 | 6.59 | 220 |
| Comparative example 2 | 86.5 | 93.7 | 5.65 | 215 |
| Comparative example 3 | 88.5 | 94.5 | 5.45 | 216 |
| Control group | 89.8 | 92.4 | 6.23 | 210 |
As seen from the experiment：The rice husk of the present invention prepares the Efficient utilization method of white carbon, by the use of rice husk as raw material, omits
The preparation process of the intermediate product of waterglass, production cost declines to a great extent, and quality is higher than the white carbon that the precipitation method are prepared,
The quality prepared with gas phase method is more or less the same.
Claims (3)
1. a kind of rice husk prepares the Efficient utilization method of white carbon, it is characterised in that comprise the following steps：
（1）It is 3-5% that rice husk, which is dried after over cleaning removal of impurities to water content, is pulverized, and 40-60 mesh sieves is crossed, into powdered rice hulls
Add mass fraction be 20-30% watery hydrochloric acid, mass fraction be 10-15% acetone, mass fraction be 5-8% ethyl acetate
And the sodium bicarbonate solution that mass fraction is 3-5%, after stirring, heating is boiled, and maintains the fluidized state of 3-4 hours,
Period is added in heating systems using deionized water, adjusts the pH value of system between 6.8-7.0；
（2）The mixed system cooked is cooled to 20-25 DEG C, filtered after standing 4-6 hours, obtained filtrate input
Into acetone soln, it is totally submerged, the stearic acid that mass fraction is 2-3% has been dissolved in acetone soln, 55-60 DEG C has been heated to, no
Disconnected stirring is vapored away completely to acetone soln, is dried in an oven to constant weight, drying temperature is 80-90 DEG C, obtained dried object；
（3）The aerosil that mass fraction is 0.3-0.5%, 20-30 points of ultrasonic disperse are added into obtained dried object
Clock, obtained dispersion is placed in Muffle furnace and is heated to 550-650 DEG C, is calcined 3-5 hours, is obtained white particulate titanium dioxide
Pulverized after silicon, cooling, spray drying produces white carbon in 1.5-2 hours at 100-110 DEG C.
2. a kind of rice husk as claimed in claim 1 prepares the Efficient utilization method of white carbon, it is characterised in that step（1）In it is dilute
The mass concentration of hydrochloric acid is 2-3%, and the mass concentration of sodium acid carbonate is 0.5-0.6%.
3. a kind of rice husk as claimed in claim 1 prepares the Efficient utilization method of white carbon, it is characterised in that step（3）Middle institute
The preparation method for stating aerosil is：Using tetraethyl orthosilicate as raw material, the water of 2-2.5 times of volume is added as solvent,
Concentration for 0.15-0.20 mol/Ls hydrochloric acid as catalyst, after mixing, be sufficiently stirred under 280-300 revs/min,
Stirring liquid is put into closed insulating box constant temperature at 60-65 DEG C to place, is taken out after after gel generation, places aging at room temperature
24-36 hours, the hydrogel after aging is replaced using supercritical carbon dioxide process and obtains aeroge.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109384237A (en) * | 2018-10-31 | 2019-02-26 | 昆明理工大学 | High-purity Si O is extracted in a kind of rice husk2Method |
| CN109467094A (en) * | 2018-12-25 | 2019-03-15 | 安徽确成硅化学有限公司 | A kind of preparation method preparing functional white carbon black using the leaf of bamboo |
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| CN103073006A (en) * | 2013-01-30 | 2013-05-01 | 化工部长沙设计研究院 | Preparation method of mesoporous silica |
| CN103508459A (en) * | 2012-06-26 | 2014-01-15 | 王金山 | Technology for producing white carbon black and active carbon from rice hull |
| WO2015186045A2 (en) * | 2014-06-03 | 2015-12-10 | Bridgedots Techservices Pvt. Ltd. | Highly dispersible precipitated silica and method of preparation thereof |
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| CN105238432A (en) * | 2015-10-20 | 2016-01-13 | 江西金糠新材料科技有限公司 | Method and device for preparing high-quality bio-oil and white carbon black through self-heating acid pickling-pyrolysis-combustion integration |
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| CN103508459A (en) * | 2012-06-26 | 2014-01-15 | 王金山 | Technology for producing white carbon black and active carbon from rice hull |
| CN103073006A (en) * | 2013-01-30 | 2013-05-01 | 化工部长沙设计研究院 | Preparation method of mesoporous silica |
| WO2015186045A2 (en) * | 2014-06-03 | 2015-12-10 | Bridgedots Techservices Pvt. Ltd. | Highly dispersible precipitated silica and method of preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109384237A (en) * | 2018-10-31 | 2019-02-26 | 昆明理工大学 | High-purity Si O is extracted in a kind of rice husk2Method |
| CN109467094A (en) * | 2018-12-25 | 2019-03-15 | 安徽确成硅化学有限公司 | A kind of preparation method preparing functional white carbon black using the leaf of bamboo |
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