CN106082240A - A kind of method utilizing starch and gangue to prepare Nano carbon white - Google Patents
A kind of method utilizing starch and gangue to prepare Nano carbon white Download PDFInfo
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- CN106082240A CN106082240A CN201610636148.3A CN201610636148A CN106082240A CN 106082240 A CN106082240 A CN 106082240A CN 201610636148 A CN201610636148 A CN 201610636148A CN 106082240 A CN106082240 A CN 106082240A
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- radix puerariae
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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
- C01B33/126—Preparation of silica of undetermined type
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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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
- C01P2006/90—Other properties not specified above
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Abstract
The present invention relates to a kind of method utilizing starch and gangue to prepare Nano carbon white, belong to white carbon preparing technical field.The present invention by manually smashing grinding to pieces to Radix Puerariae, water washing and precipitating obtains Radix Puerariae starch, thicker sodium silicate shrend after gangue and soda mixing congruent melting obtained, and utilizes high pressure to be dissolved in deionized water, acid hydrolysis also adds Radix Puerariae starch absorption silicon dioxide, i.e. obtains Nano carbon white after calcining.Nano carbon white prepared by the present invention is difficult to reunite, and particle dispersive property is good, and N2 adsorption specific surface area is 175～200m2/g；And preparation technology is simple, preparation process energy consumption is low, required low cost.
Description
Technical field
The present invention relates to a kind of method utilizing starch and gangue to prepare Nano carbon white, belong to white carbon technology of preparing neck
Territory.
Background technology
White carbon i.e. amorphous silicon di-oxide, molecular formula is SiO2·nH2O, is a kind of fine powdery white, nontoxic, unformed
Thing, has porous, polymolecularity, light weight, the excellent properties such as chemical stability is good, high temperature resistant, do not burn and electrical insulating property is good.
The preparation method of white carbon has a lot, and wherein nonmetallic ore method is to prepare the new method of white carbon.Nonmetallic ore method be with rich in
Nonmetallic ore be raw material, by chemical method, the silicon dioxide of crystalline state is changed into amorphous carbon/silicon dioxide, thus makes
Ultra-fine, the white carbon of high-specific surface area of different requirement must be met.
Gangue is and the rock of coal association, is the solid slag being separated in the processing of colliery, is multiple ore deposit
The mixture of thing rock composition, is one of maximum industrial solid castoff of China current discharge capacity, for raw coal output 15%～
20%, and discharge capacity is still increasing year by year.A large amount of gangues are discharged, and both accounted for substantial amounts of arable land, and some gangue is easy simultaneously
Combustion, serious environment pollution, crops and the mankind are all worked the mischief.Along with the reach of science, people gradually recognize gangue
Also it is available a kind of resource.In recent years, China expands gangue comprehensive utilizating research in various fields, wherein with bastard coal
Stone is that primary raw material prepares white carbon, has good economic benefit and social benefit.White carbon is the nothing with greater activity
Setting SiO2, have a wide range of applications in industries such as tire, latex, plastics, cosmetics, papermaking and fertilizer.
Owing to Nano carbon white has greatly specific surface area and surface energy, owing to generally existing between particle in preparation process
Van der Waals force, Coulomb force even chemical bond, easily reunite so that powder particle can not be uniform with nanometer grade
And stable dispersion, when causing applying, due performance reduces or loses.
Summary of the invention
The technical problem to be solved: have great specific surface area and surface energy for Nano carbon white, preparing
Due to the Van der Waals force generally existed between particle, Coulomb force even chemical bond in journey, easily reunite so that powder body
Particle can not be with nanometer grade uniformly stable dispersion, the defect that when causing applying, due performance reduces or loses, this
Bright by Radix Puerariae is manually smashed to pieces grinding, water washing and precipitating obtains Radix Puerariae starch, then by after gangue and soda mixing congruent melting
The thick sodium silicate that shrend obtains, utilizes high pressure to be dissolved in deionized water, and acid hydrolysis also adds Radix Puerariae starch absorption titanium dioxide
Silicon, i.e. obtains Nano carbon white after calcining.The present invention polyhydroxy characteristic by Radix Puerariae starch, with sodium silicate solution hydrolysis precipitation
White carbon surface produces chemical bond and physical absorption, is arranged in starch particle surface uniformly, decreases the model moral of Linesless charcoal night
Hua Li, prevents them to attract each other and the phenomenon reunited occurs, after be pyrolyzed starch through high-temperature calcination, i.e. can get nanometer white
White carbon black, the present invention solves in tradition white carbon preparation process and easily reunites so that powder particle can not be with nanometer grade
Uniformly stable dispersion, the problem that when causing applying, performance reduces or loses, there is wide prospect of production.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
(1) weigh 2～3kg Radix Puerariaes to put in ultrasonic cleaning instrument with 200～300W power cleanings 10～15min, take out after cleaning
Radix Puerariae naturally dry, the Radix Puerariae after drying manually is cut into the segment of 5～8cm, then puts in stone mortar by the segment obtained, use
Grinding 1～2h smashed to pieces by stone pestle；
(2), after end to be ground, with the Radix Puerariae after smashing to pieces in 8～10L deionized water rinsing stone mortars, milky flushing liquor is collected also
It is loaded in ceramic pot, stands overnight in the ice-water bath of 4～6 DEG C, separate and remove the supernatant, obtain bottom pasty state Radix Puerariae
Starch slurry, is finally putting in 40～50 DEG C of baking ovens and is dried 7～8h, obtain Radix Puerariae starch, standby；
(3) weigh 2～3kg gangues and put in ball mill, be that 30:1 adds stainless steel ball-milling pearl in ball grinder by ratio of grinding media to material,
Grinding terminates rear discharging and crosses 150 mesh standard sieves and obtain gangue powder, then is 1 by gangue powder and sodium carbonate by quality:
Putting into Muffle furnace after 40 mix homogeneously together, be warming up to 800～900 DEG C with 5 DEG C/min rate program, blended smelting melts 1～2h；
(4) after smelting clinkering bundle, fused mass is poured into immediately shrend in boiling water, is filtrated to get thick sodium silicate solids, puts it into
In autoclave, add thick sodium silicate solids quality 3～the distilled water of 5 times, 8～10MPa and the bar of 120～150 DEG C
Stirring and dissolving 6～8h under part, filter to separate and remove filtering residue, obtain sodium silicate solution；
(5) adding equal-volume mass concentration in above-mentioned sodium silicate solution is 5% sulfuric acid solution, acidleach 8～10h under room temperature, then uses
Concentration is that 0.3mol/L sodium hydroxide solution regulates pH to 7.0～7.5, then is that 1:5 adds standby Radix Puerariae inwards by solid-to-liquid ratio
Starch, is warming up to 50～55 DEG C of insulation ripenings 20～30min, pours product into buchner funnel, use deionized water after stirring
Filtering and washing 3～obtain filtering residue 5 times；
(6) filtering residue obtained above is put in Muffle furnace, be warming up to 400～500 DEG C with 3～5 DEG C/min rate program, insulation
Discharging after calcining 2～3h, the white powder obtained is Nano carbon white.
Nano carbon white N2 adsorption specific surface area prepared by the present invention is 175～200m2/ g, 500% stress at definite elongation is
More than 7.5MPa, elongation rate of tensile failure is more than 820%, and hot strength is 2.3～3.4cm more than 25MPa, DBP absorption value2/g。
The present invention is compared with additive method, and Advantageous Effects is:
(1) Nano carbon white prepared by the present invention be difficult to reunite, particle dispersive property is good, N2 adsorption specific surface area be 175～
200m2/g；
(2) the Nano carbon white preparation technology that prepared by the present invention is simple, and preparation process energy consumption is low, required low cost.
Detailed description of the invention
First weigh 2～3kg Radix Puerariaes to put in ultrasonic cleaning instrument with 200～300W power cleanings 10～15min, take out clear
Radix Puerariae after washing dries naturally, and the Radix Puerariae after drying manually is cut into the segment of 5～8cm, then the segment obtained is put into stone mortar
In, smash grinding 1～2h to pieces with stone pestle；After end to be ground, with the Radix Puerariae after smashing to pieces in 8～10L deionized water rinsing stone mortars, receive
Collection milky flushing liquor is also loaded in ceramic pot, stands overnight in the ice-water bath of 4～6 DEG C, separates and removes the supernatant,
Obtain bottom pasty state Radix Puerariae starch slurry, be finally putting in 40～50 DEG C of baking ovens and be dried 7～8h, obtain Radix Puerariae starch, standby；Weigh again
2～3kg gangues are put in ball mill, are that 30:1 adds stainless steel ball-milling pearl in ball grinder by ratio of grinding media to material, grind after terminating
Discharging is also crossed 150 mesh standard sieves and is obtained gangue powder, then is 1:40 mix homogeneously by gangue powder and sodium carbonate by quality
After put into Muffle furnace together, be warming up to 800～900 DEG C with 5 DEG C/min rate program, blended smelting melts 1～2h；
After smelting clinkering bundle, fused mass is poured into immediately shrend in boiling water, is filtrated to get thick sodium silicate solids, puts it into high pressure
In reactor, add thick sodium silicate solids quality 3～the distilled water of 5 times, under conditions of 8～10MPa and 120～150 DEG C
Stirring and dissolving 6～8h, filters to separate and removes filtering residue, obtain sodium silicate solution；Then the body such as addition in above-mentioned sodium silicate solution
Long-pending mass concentration is 5% sulfuric acid solution, acidleach 8～10h under room temperature, then is that 0.3mol/L sodium hydroxide solution regulates pH by concentration
To 7.0～7.5, then it is that 1:5 adds standby Radix Puerariae starch inwards by solid-to-liquid ratio, after stirring, is warming up to 50～55 DEG C of insulations
Ripening 20～30min, pours product into buchner funnel, obtains filtering residue by deionized water filtering and washing 3～5 times；Finally by above-mentioned
The filtering residue obtained is put in Muffle furnace, is warming up to 400～500 DEG C with 3～5 DEG C/min rate program, goes out after insulation calcining 2～3h
Material, the white powder obtained is Nano carbon white.
Example 1
First weigh 3kg Radix Puerariae to put in ultrasonic cleaning instrument with 300W power cleaning 15min, take out the Radix Puerariae after cleaning and naturally dry in the air
Dry, the Radix Puerariae after drying manually is cut into the segment of 8cm, then puts in stone mortar by the segment obtained, and smashs grinding 2h to pieces with stone pestle；
After end to be ground, with the Radix Puerariae after smashing to pieces in 10L deionized water rinsing stone mortar, collect milky flushing liquor and be also loaded into pottery
In porcelain jar, stand overnight in the ice-water bath of 6 DEG C, separate and remove the supernatant, obtain bottom pasty state Radix Puerariae starch slurry, finally put
Enter and 50 DEG C of baking ovens are dried 8h, obtain Radix Puerariae starch, standby；Weigh 3kg gangue again and put in ball mill, be 30:1 by ratio of grinding media to material
In ball grinder, add stainless steel ball-milling pearl, grind and terminate rear discharging and cross 150 mesh standard sieves to obtain gangue powder, then by coal
Spoil powder be 1:40 mix homogeneously with sodium carbonate by quality after together with put into Muffle furnace, be warming up to 5 DEG C/min rate program
900 DEG C, 2h is melted in blended smelting；After smelting clinkering bundle into, fused mass is poured immediately shrend in boiling water, be filtrated to get thick sodium silicate solid
Body, puts it in autoclave, adds the distilled water of thick sodium silicate solids quality 5 times, at 10MPa and the bar of 150 DEG C
Stirring and dissolving 8h under part, filters to separate and removes filtering residue, obtain sodium silicate solution；Then the body such as addition in above-mentioned sodium silicate solution
Long-pending mass concentration is 5% sulfuric acid solution, acidleach 10h under room temperature, then is that 0.3mol/L sodium hydroxide solution regulates pH extremely by concentration
7.5, then be that 1:5 adds standby Radix Puerariae starch inwards by solid-to-liquid ratio, it is warming up to 55 DEG C of insulation ripening 30min after stirring,
Pour product into buchner funnel, obtain filtering residue 5 times by deionized water filtering and washing；Finally filtering residue obtained above is put into Muffle
In stove, being warming up to 500 DEG C with 5 DEG C/min rate program, discharging after insulation calcining 3h, the white powder obtained is nanometer Linesless charcoal
Black.
After testing, the Nano carbon white N2 adsorption specific surface area that prepared by the present invention is 200m2/ g, 500% stress at definite elongation is
7.8MPa, elongation rate of tensile failure is 825%, hot strength be 26MPa, DBP absorption value be 3.4cm2/g。
Example 2
First weigh 2kg Radix Puerariae to put in ultrasonic cleaning instrument with 200W power cleaning 10min, take out the Radix Puerariae after cleaning and naturally dry in the air
Dry, the Radix Puerariae after drying manually is cut into the segment of 5cm, then puts in stone mortar by the segment obtained, and smashs grinding 1h to pieces with stone pestle；
After end to be ground, with the Radix Puerariae after smashing to pieces in 8L deionized water rinsing stone mortar, collect milky flushing liquor and be also loaded into pottery
In porcelain jar, stand overnight in the ice-water bath of 4 DEG C, separate and remove the supernatant, obtain bottom pasty state Radix Puerariae starch slurry, finally put
Enter and 40 DEG C of baking ovens are dried 7h, obtain Radix Puerariae starch, standby；Weigh 2kg gangue again and put in ball mill, be 30:1 by ratio of grinding media to material
In ball grinder, add stainless steel ball-milling pearl, grind and terminate rear discharging and cross 150 mesh standard sieves to obtain gangue powder, then by coal
Spoil powder be 1:40 mix homogeneously with sodium carbonate by quality after together with put into Muffle furnace, be warming up to 5 DEG C/min rate program
800 DEG C, 1h is melted in blended smelting；After smelting clinkering bundle into, fused mass is poured immediately shrend in boiling water, be filtrated to get thick sodium silicate solid
Body, puts it in autoclave, adds the distilled water of thick sodium silicate solids quality 3 times, in 8MPa and the condition of 120 DEG C
Lower stirring and dissolving 6h, filters to separate and removes filtering residue, obtain sodium silicate solution；Then in above-mentioned sodium silicate solution, add equal-volume
Mass concentration is 5% sulfuric acid solution, acidleach 8h under room temperature, then is that 0.3mol/L sodium hydroxide solution regulates pH to 7.0 by concentration,
It is that 1:5 adds standby Radix Puerariae starch inwards by solid-to-liquid ratio again, is warming up to 50 DEG C of insulation ripening 20min after stirring, will produce
Thing pours buchner funnel into, obtains filtering residue 3 times by deionized water filtering and washing；Finally filtering residue obtained above is put into Muffle furnace
In, it being warming up to 400 DEG C with 3 DEG C/min rate program, discharging after insulation calcining 2h, the white powder obtained is nanometer Linesless charcoal
Black.
Nano carbon white N2 adsorption specific surface area prepared by the present invention is 175m2/ g, 500% stress at definite elongation is 7.7MPa,
Elongation rate of tensile failure is 830%, hot strength be 30MPa, DBP absorption value be 2.3cm2/g。
Example 3
First weigh 2.5kg Radix Puerariae to put in ultrasonic cleaning instrument with 250W power cleaning 12min, take out the Radix Puerariae after cleaning natural
Drying, the Radix Puerariae after drying manually is cut into the segment of 6cm, then puts in stone mortar by the segment obtained, and smashs grinding to pieces with stone pestle
2h；After end to be ground, with the Radix Puerariae after smashing to pieces in 9L deionized water rinsing stone mortar, collect milky flushing liquor and be also loaded into
In ceramic pot, stand overnight in the ice-water bath of 5 DEG C, separate and remove the supernatant, obtain bottom pasty state Radix Puerariae starch slurry, finally
Put into and 45 DEG C of baking ovens are dried 7h, obtain Radix Puerariae starch, standby；Weigh 2.5kg gangue again and put in ball mill, by ratio of grinding media to material be
30:1 adds stainless steel ball-milling pearl in ball grinder, grinds and terminates rear discharging and cross 150 mesh standard sieves to obtain gangue powder, then
Muffle furnace is put into, with 5 DEG C/min rate program liter together with after being 1:40 mix homogeneously with sodium carbonate by quality by gangue powder
Temperature is to 850 DEG C, and 2h is melted in blended smelting；After smelting clinkering bundle, fused mass is poured into immediately shrend in boiling water, is filtrated to get thick sodium silicate
Solid, puts it in autoclave, adds the distilled water of thick sodium silicate solids quality 4 times, at 9MPa and the bar of 130 DEG C
Stirring and dissolving 7h under part, filters to separate and removes filtering residue, obtain sodium silicate solution；Then the body such as addition in above-mentioned sodium silicate solution
Long-pending mass concentration is 5% sulfuric acid solution, acidleach 9h under room temperature, then is that 0.3mol/L sodium hydroxide solution regulates pH extremely by concentration
7.2, then be that 1:5 adds standby Radix Puerariae starch inwards by solid-to-liquid ratio, it is warming up to 52 DEG C of insulation ripening 25min after stirring,
Pour product into buchner funnel, obtain filtering residue 4 times by deionized water filtering and washing；Finally filtering residue obtained above is put into Muffle
In stove, being warming up to 450 DEG C with 4 DEG C/min rate program, discharging after insulation calcining 3h, the white powder obtained is nanometer Linesless charcoal
Black.
Nano carbon white N2 adsorption specific surface area prepared by the present invention is 180m2/ g, 500% stress at definite elongation is 7.8MPa,
Elongation rate of tensile failure is 830%, hot strength be 28MPa, DBP absorption value be 3.1cm2/g。
Claims (1)
1. one kind utilizes the method that starch and gangue prepare Nano carbon white, it is characterised in that concrete preparation process is:
(1) weigh 2～3kg Radix Puerariaes to put in ultrasonic cleaning instrument with 200～300W power cleanings 10～15min, take out after cleaning
Radix Puerariae naturally dry, the Radix Puerariae after drying manually is cut into the segment of 5～8cm, then puts in stone mortar by the segment obtained, use
Grinding 1～2h smashed to pieces by stone pestle；
(2), after end to be ground, with the Radix Puerariae after smashing to pieces in 8～10L deionized water rinsing stone mortars, milky flushing liquor is collected also
It is loaded in ceramic pot, stands overnight in the ice-water bath of 4～6 DEG C, separate and remove the supernatant, obtain bottom pasty state Radix Puerariae
Starch slurry, is finally putting in 40～50 DEG C of baking ovens and is dried 7～8h, obtain Radix Puerariae starch, standby；
(3) weigh 2～3kg gangues and put in ball mill, be that 30:1 adds stainless steel ball-milling pearl in ball grinder by ratio of grinding media to material,
Grinding terminates rear discharging and crosses 150 mesh standard sieves and obtain gangue powder, then is 1 by gangue powder and sodium carbonate by quality:
Putting into Muffle furnace after 40 mix homogeneously together, be warming up to 800～900 DEG C with 5 DEG C/min rate program, blended smelting melts 1～2h；
(4) after smelting clinkering bundle, fused mass is poured into immediately shrend in boiling water, is filtrated to get thick sodium silicate solids, puts it into
In autoclave, add thick sodium silicate solids quality 3～the distilled water of 5 times, 8～10MPa and the bar of 120～150 DEG C
Stirring and dissolving 6～8h under part, filter to separate and remove filtering residue, obtain sodium silicate solution；
(5) adding equal-volume mass concentration in above-mentioned sodium silicate solution is 5% sulfuric acid solution, acidleach 8～10h under room temperature, then uses
Concentration is that 0.3mol/L sodium hydroxide solution regulates pH to 7.0～7.5, then is that 1:5 adds standby Radix Puerariae inwards by solid-to-liquid ratio
Starch, is warming up to 50～55 DEG C of insulation ripenings 20～30min, pours product into buchner funnel, use deionized water after stirring
Filtering and washing 3～obtain filtering residue 5 times；
(6) filtering residue obtained above is put in Muffle furnace, be warming up to 400～500 DEG C with 3～5 DEG C/min rate program, insulation
Discharging after calcining 2～3h, the white powder obtained is Nano carbon white.
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| CN201610636148.3A CN106082240B (en) | 2016-08-05 | 2016-08-05 | A kind of method that Nano carbon white is prepared using starch and gangue |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174168A (en) * | 1996-08-15 | 1998-02-25 | 鞠馥阳 | Production process of active silica white from gangue |
| CN101190949A (en) * | 2006-11-30 | 2008-06-04 | 贾启海 | Technique for extracting and preparing kudzu root and fern root starch |
| CN101704525A (en) * | 2009-11-23 | 2010-05-12 | 中煤平朔煤业有限责任公司 | Preparation method of high-quality white carbon black for rubber |
| CN102226237A (en) * | 2011-05-12 | 2011-10-26 | 杨暖 | Method for extracting ammonium metavanadate, silica white and coal powder from vanadium-containing coal gangue |
| CN105747080A (en) * | 2016-03-03 | 2016-07-13 | 丁玉琴 | Method for preparing nitroso hemoglobin pigment easy to disperse and high in thermal stability |
-
2016
- 2016-08-05 CN CN201610636148.3A patent/CN106082240B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174168A (en) * | 1996-08-15 | 1998-02-25 | 鞠馥阳 | Production process of active silica white from gangue |
| CN101190949A (en) * | 2006-11-30 | 2008-06-04 | 贾启海 | Technique for extracting and preparing kudzu root and fern root starch |
| CN101704525A (en) * | 2009-11-23 | 2010-05-12 | 中煤平朔煤业有限责任公司 | Preparation method of high-quality white carbon black for rubber |
| CN102226237A (en) * | 2011-05-12 | 2011-10-26 | 杨暖 | Method for extracting ammonium metavanadate, silica white and coal powder from vanadium-containing coal gangue |
| CN105747080A (en) * | 2016-03-03 | 2016-07-13 | 丁玉琴 | Method for preparing nitroso hemoglobin pigment easy to disperse and high in thermal stability |
Non-Patent Citations (1)
| Title |
|---|
| 刘佳音: "淀粉改性白炭黑/丁苯橡胶复合材料的研究", 《中国优秀硕士学位论文全文数据库》 * |
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