CN110078081A - A method of amorphous silica is prepared using water hyacinth - Google Patents
A method of amorphous silica is prepared using water hyacinth Download PDFInfo
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- CN110078081A CN110078081A CN201910367147.7A CN201910367147A CN110078081A CN 110078081 A CN110078081 A CN 110078081A CN 201910367147 A CN201910367147 A CN 201910367147A CN 110078081 A CN110078081 A CN 110078081A
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- water hyacinth
- amorphous silica
- silica
- room temperature
- preparing amorphous
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 25
- 240000003826 Eichhornia crassipes Species 0.000 title description 2
- 241000169203 Eichhornia Species 0.000 claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000013505 freshwater Substances 0.000 claims abstract description 8
- 239000007790 solid phase Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 244000144992 flock Species 0.000 claims abstract description 6
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000000706 filtrate Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000007781 pre-processing Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 9
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 6
- 238000006297 dehydration reaction Methods 0.000 description 6
- 238000005554 pickling Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 229910018557 Si O Inorganic materials 0.000 description 4
- 229910002808 Si–O–Si Inorganic materials 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 238000004566 IR spectroscopy Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910002026 crystalline silica Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
Abstract
The present invention discloses a kind of method for preparing amorphous silica using water hyacinth, this method is by fresh water hyacinth by pre-processing, it after high-temperature calcination is cooled to room temperature at ash, is mixed with hydrochloric acid solution, 120~180min is stirred at room temperature, it is centrifugated out solid phase, after distilling water washing to neutrality, is mixed with sodium hydroxide solution, mixture is placed in heating stirring in oil bath, filtering, it is 5~7 that hydrochloric acid solution is added in filtrate and adjusts pH;It is aged 24~48h at room temperature, white flock precipitate occurs, unbodied silica is obtained after being filtered, washed and dried;The method of the present invention solves the problem of that water hyacinth overflows and destroys domestic ecosystem balance;New approach is opened up for the production of silica, achievees the effect that turn waste into wealth, realizes the requirement of environmentally friendly low-carbon.
Description
Technical field
The invention belongs to biomass high price value utilize technical field, and in particular to it is a kind of using water hyacinth prepare it is amorphous
The method of silica.
Background technique
Water hyacinth (Eichhornia crassipes) is a kind of floating plant for being grown on South America, since it is with water purification and enjoying value, two
Ten beginnings of the century were artificially induced to China;But the China domestic natural enemy for lacking this kind of plant, and water hyacinth seed survival
Time is long, reproduction speed is fast, and causing it, more ground quantity explosion type increases at home, brings eutrophication, the water of rivers and lakes
The problems such as death of biology and navigation channel blocking;Seriously destroy local ecosystem balance and diversity of organism.
Water hyacinth can be used for biomass fuel, and burn generated ash content inorganic oxide containing there are many, wherein with two
The content of silica is most, usually less than 60wt%.Silica can be divided into crystalline state and amorphous two major classes again;Titanium dioxide
Silicon is widely used for the manufacturing of the industrial products such as ceramics, refractory material, cement and glass;Amorphous silica is in high temperature
Under the conditions of be soluble in lye and form sodium silicate solution, i.e. waterglass;And crystalline silica is not easy to form sodium silicate solution;Nothing
Amorphous silicon dioxide is both synthesis of molecular sieve and prepares the indispensable raw material of silica gel adsorptive material;It is burnt using water hyacinth
The ash content of generation prepares amorphous silica, has saved the cost of production amorphous silica and its accessory, at present state
Inside and outside relevant research is also less.
Summary of the invention
In view of the problems of the existing technology and insufficient, the present invention, which provides, a kind of prepares amorphous titanium dioxide using water hyacinth
The method of silicon, it is intended to solve the problem of that water hyacinth overflows and destroy domestic ecosystem balance;It is opened for the production of silica
New approach is warded off, achievees the effect that turn waste into wealth, realizes the requirement of environmentally friendly low-carbon.
The method of the present invention is by fresh water hyacinth by pre-processing, molten with hydrochloric acid after high-temperature calcination is cooled to room temperature at ash
Liquid mixing, is stirred at room temperature 120~180min, is centrifugated out solid phase, mixed with sodium hydroxide solution after distilling water washing to neutrality
It closes, mixture is placed in heating stirring in oil bath, filter, it is 5~7 that hydrochloric acid solution is added in filtrate and adjusts pH;It is old at room temperature
Change 24~48h, white flock precipitate occurs, unbodied silica is obtained after being filtered, washed and dried;
The concrete operations of the above method are as follows: fresh water hyacinth pulverizer is crushed and natural drying is to after being dehydrated, 500~
120~360min is calcined at 700 DEG C, is cooled to room temperature;The ratio that 20~50mL is added in every 1g water hyacinth ash, by water hyacinth ash
It is mixed with the hydrochloric acid solution of 5~6mol/L of concentration, 120~180min is stirred at room temperature, the centrifugation point at 5000~6000rpm
Solid phase is separated out, after solid phase is washed with distilled water to neutrality, the ratio of 40~60mL is added in every 1g solid phase, is by solid phase and concentration
The sodium hydroxide solution of 1.0~1.5mol/L mixes, and mixture is placed in 12~20h of stirring, vacuum in 200~300 DEG C of oil baths
Under the conditions of filter, in filtrate be added hydrochloric acid solution adjust pH be 5~7;It is aged 24~48h at room temperature, it is heavy white flock occur
It forms sediment, unbodied silica is made at residue washing and 80~100 DEG C after dry 8~10h in filtering.
The beneficial effects of the present invention are:
1, in the method for the present invention, water hyacinth belongs to exotic invasive floating plant, meets the theme of ecological protection;
2, the method that the preparation of amorphous silica mainly takes alkali-soluble acid analysis in the method for the present invention, easy to operate, gained produces
The activation of product silica is uniformly, with high purity;
3, water hyacinth distributed number is more in the method for the present invention, and reproduction speed is fast, and raw material sources are extensive.
Detailed description of the invention
Fig. 1 is the XRD diagram of amorphous silica prepared by the embodiment of the present invention 1;
Fig. 2 is infrared spectroscopy (FTIR) figure of amorphous silica prepared by the embodiment of the present invention 1;
Fig. 3 is the pictorial diagram of amorphous silica prepared by the embodiment of the present invention 1.
Specific embodiment
Embodiment 1: this is to take fresh water hyacinth 1kg using the method that water hyacinth prepares amorphous silica, with crushing
Machine is ground into fine particle, is placed under sunlight and dries 6 days until dehydration;Dehydration water hyacinth is placed in Muffle furnace and is heated to 600
DEG C, high-temperature calcination 250min is cooled to room temperature (grey chemical component is shown in Table 1 after calcining);100mL is added in 5g water hyacinth ash
6mol/L hydrochloric acid solution, the at the uniform velocity ash content that is generated with pickling of stirring 120min at room temperature, a small amount of metal that removing wherein contains
Oxide;Grey black after being centrifugated out pickling at 6000rpm is washed repeatedly with distilled water to neutrality;Add by every 1g grey black
The ratio for adding 50mL sodium hydroxide solution mixes grey black with the 1.0mol/L sodium hydroxide solution of 200mL, in 240 DEG C of oil baths
In at the uniform velocity stir 12 hours, filtrate pH is adjusted to 6 with 6mol/L hydrochloric acid solution, is aged at room temperature by the filtrate of vacuum filtration
For 24 hours, there is white flock precipitate, filter, after distillation water washing, it is 8 hours dry at 100 DEG C, obtain white-amorphous dioxy
SiClx solid particle;
Table 1: the main chemical compositions (wt%) of water hyacinth ash
XRD, FTIR characterization are carried out to silica manufactured in the present embodiment, as a result such as Fig. 1 to Fig. 2;From figure 1 it appears that
The diffraction peak of the diffraction maximum position of silica manufactured in the present embodiment and intensity with amorphous silica standard spectrogram
It sets and intensity is coincide substantially, show that substance manufactured in the present embodiment is amorphous silica;By analyzing Fig. 2 it is found that originally
The silica of embodiment preparation has typical Si-O, Si-O-Si structure, wherein 1090cm-1The absorption peak of Qiang Erkuan belongs to
Si-O-Si antisymmetric stretching vibration, 795cm-1、464cm-1The absorption peak at place belongs to Si-O symmetrical stretching vibration and bending vibration,
3450cm-1The broad peak at place belongs to the antisymmetric stretching vibration peak of hydroxyl in constitution water, 1638cm-1The absorption peak at place belongs to H-O-H
Flexural vibrations peak;Fig. 3 is the pictorial diagram for preparing amorphous silica, has the complexion feature of silica.
Embodiment 2: it is to take fresh water hyacinth 1kg using the method that water hyacinth prepares amorphous silica, uses pulverizer
It is ground into fine particle, is placed under sunlight and dries 6 days until dehydration;Dehydration water hyacinth is placed in Muffle furnace and is heated to 700 DEG C,
High-temperature calcination 180min is cooled to room temperature (grey chemical component is shown in Table 2 after calcining);Add 150mL's in 5g water hyacinth ash
5mol/L hydrochloric acid solution, the ash content that at the uniform velocity stirring 150min is generated at room temperature with pickling, removes a small amount of metal oxygen wherein contained
Compound;Grey black after being centrifugated out pickling at 5000rpm is washed repeatedly with distilled water to neutrality;It is added by every 1g grey black
Grey black is mixed with 1.2mol/L sodium hydroxide solution, is at the uniform velocity stirred in 200 DEG C of oil baths by the ratio of 60mL sodium hydroxide solution
Filtrate pH is adjusted to 5 with 6mol/L hydrochloric acid solution, is aged 30h at room temperature, white flock occur by 20h, the filtrate of vacuum filtration
Precipitating filters, after distillation water washing, 10 hours dry at 80 DEG C, obtains white, amorphous silica solid particle;
Table 2: the main chemical compositions (wt%) of water hyacinth ash
XRD, FTIR characterization are carried out to amorphous silica manufactured in the present embodiment, the results showed that nothing manufactured in the present embodiment is fixed
The XRD diffraction maximum position of shape silica and intensity with the diffraction maximum position of amorphous silica standard spectrogram and rheobase
This coincide, and shows that substance manufactured in the present embodiment is amorphous silica;Amorphous silica manufactured in the present embodiment
Infrared spectroscopy (FTIR) spectrogram is similar to Fig. 2 of embodiment 1, and the silica of preparation is tied with typical Si-O, Si-O-Si
Structure further proves that the product synthesized is amorphous silica;Meanwhile the amorphous silica that the present embodiment is prepared
Pictorial diagram is similar to Fig. 3 of embodiment 1, has the complexion feature of silica.
Embodiment 3: it is to take fresh water hyacinth 1kg using the method that water hyacinth prepares amorphous silica, uses pulverizer
It is ground into fine particle, is placed under sunlight and dries 6 days until dehydration;Dehydration water hyacinth is placed in Muffle furnace and is heated to 500 DEG C,
High-temperature calcination 350min is cooled to room temperature (grey chemical component is shown in Table 3 after calcining);Add 200mL's in 5g water hyacinth ash
5.5mol/L hydrochloric acid solution, the ash content that at the uniform velocity stirring 150min is generated at room temperature with pickling, removes a small amount of metal wherein contained
Oxide;Grey black after being centrifugated out pickling at 5500rpm is washed repeatedly with distilled water to neutrality;Add by every 1g grey black
Grey black is mixed with 1.5mol/L sodium hydroxide solution, is at the uniform velocity stirred in 300 DEG C of oil baths by the ratio for adding 40mL sodium hydroxide solution
12h is mixed, filtrate pH is adjusted to 7 with 6mol/L hydrochloric acid solution by the filtrate of vacuum filtration, is aged 40h at room temperature, white wadding occurs
Shape precipitating filters, after distillation water washing, 9 hours dry at 90 DEG C, obtains white, amorphous silica solid particle;
Table 3: the main chemical compositions (wt%) of water hyacinth ash
XRD, FTIR characterization are carried out to amorphous silica manufactured in the present embodiment, the results showed that nothing manufactured in the present embodiment is fixed
The XRD diffraction maximum position of shape silica and intensity with the diffraction maximum position of amorphous silica standard spectrogram and rheobase
This coincide, and shows that substance manufactured in the present embodiment is amorphous silica;Amorphous silica manufactured in the present embodiment
Infrared spectroscopy (FTIR) spectrogram is similar to Fig. 2 of embodiment 1, and the silica of preparation is tied with typical Si-O, Si-O-Si
Structure further proves that the product synthesized is amorphous silica;Meanwhile the amorphous silica that the present embodiment is prepared
Pictorial diagram is similar to Fig. 3 of embodiment 1, has the complexion feature of silica.
Claims (8)
1. a kind of method for preparing amorphous silica using water hyacinth, it is characterised in that: by fresh water hyacinth by pre- place
Reason, after high-temperature calcination is cooled to room temperature at ash, mixes with hydrochloric acid solution, 120~180min is stirred at room temperature, and is centrifugated out solid
Phase mixes with sodium hydroxide solution after distilling water washing to neutrality, mixture is placed in heating stirring in oil bath, filters, is filtering
It is 5~7 that hydrochloric acid solution is added in liquid and adjusts pH;It is aged 24~48h at room temperature, white flock precipitate occurs, is filtered, washed and does
Unbodied silica is obtained after dry.
2. the method according to claim 1 for preparing amorphous silica using water hyacinth, it is characterised in that: fresh water
Cucurbit pretreatment is extremely dehydrated to crush with natural drying.
3. the method according to claim 1 for preparing amorphous silica using water hyacinth, it is characterised in that: calcining is
120~360min is handled at 500~700 DEG C.
4. the method according to claim 1 for preparing amorphous silica using water hyacinth, it is characterised in that: hydrochloric acid is molten
The concentration of liquid is 5~6mol/L, adds hydrochloric acid solution in the ratio that every 1g water hyacinth ash adds 20~50mL.
5. the method according to claim 1 for preparing amorphous silica using water hyacinth, it is characterised in that: centrifugation turns
Speed is 5000~6000rpm.
6. the method according to claim 1 for preparing amorphous silica using water hyacinth, it is characterised in that: hydroxide
The concentration of sodium solution is 1.0~1.5mol/L, adds sodium hydroxide solution in the ratio that every 1g solid phase adds 40~60mL.
7. the method according to claim 1 for preparing amorphous silica using water hyacinth, it is characterised in that: in oil bath
Heating stirring is 12~20h of stirring at 200~300 DEG C.
8. the method according to claim 1 for preparing amorphous silica using water hyacinth, it is characterised in that: dry temperature
Degree is 80~100 DEG C, and the time is 8~10h.
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