CN109665534A - A method of mesopore silicon oxide is prepared using flyash acid leaching residue - Google Patents
A method of mesopore silicon oxide is prepared using flyash acid leaching residue Download PDFInfo
- Publication number
- CN109665534A CN109665534A CN201811395289.6A CN201811395289A CN109665534A CN 109665534 A CN109665534 A CN 109665534A CN 201811395289 A CN201811395289 A CN 201811395289A CN 109665534 A CN109665534 A CN 109665534A
- Authority
- CN
- China
- Prior art keywords
- acid leaching
- fly ash
- mesoporous silica
- concentration
- leaching slag
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000010881 fly ash Substances 0.000 title claims abstract description 40
- 238000002386 leaching Methods 0.000 title claims abstract description 36
- 239000002253 acid Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910052814 silicon oxide Inorganic materials 0.000 title description 21
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000012065 filter cake Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- QPILZZVXGUNELN-UHFFFAOYSA-N sodium;4-amino-5-hydroxynaphthalene-2,7-disulfonic acid Chemical compound [Na+].OS(=O)(=O)C1=CC(O)=C2C(N)=CC(S(O)(=O)=O)=CC2=C1 QPILZZVXGUNELN-UHFFFAOYSA-N 0.000 claims abstract 11
- 239000002893 slag Substances 0.000 claims abstract 10
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000004115 Sodium Silicate Substances 0.000 claims description 13
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 13
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 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 description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 230000007935 neutral effect Effects 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 abstract 1
- 235000011941 Tilia x europaea Nutrition 0.000 abstract 1
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- 239000004571 lime Substances 0.000 abstract 1
- 239000001488 sodium phosphate Substances 0.000 abstract 1
- 229910000162 sodium phosphate Inorganic materials 0.000 abstract 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 239000002994 raw material Substances 0.000 description 7
- 239000000908 ammonium hydroxide Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000006004 Quartz sand Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000010883 coal ash Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- 229910003978 SiClx 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
-
- 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
-
- 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
- C01P2006/16—Pore diameter
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
本发明公开了一种利用粉煤灰酸浸渣制备介孔氧化硅的方法，包括以下步骤：1)粉煤灰与硫酸或盐酸在120～140℃下酸浸后，过滤分离，得到粉煤灰酸浸渣；2)将粉煤灰酸浸渣与氢氧化钠溶液按照固液比1:2～1:4混合，在60～90℃下溶解反应0.5～2h，趁热过滤，得到高模数水玻璃；3)调整水玻璃中硅的浓度，用硫酸调节溶液的pH值为4～5，反应5～10min；4)用氨水调节溶胶的pH值为7～9，再加入六偏磷酸钠，在30～60℃下老化0.5～2h；5)将老化后的混合物进行固液分离，得到滤饼；6)将滤饼在100～110℃下干燥1～2h，再在300～400℃下焙烧1.5～3h，冷却后得到介孔氧化硅。
The invention discloses a method for preparing mesoporous silica by using fly ash acid leaching slag. Lime acid leaching residue; 2) Mix the fly ash acid leaching slag and sodium hydroxide solution according to the solid-liquid ratio of 1:2 to 1:4, dissolve and react at 60 to 90 ° C for 0.5 to 2 hours, and filter while hot to obtain high Modulus water glass; 3) Adjust the concentration of silicon in the water glass, use sulfuric acid to adjust the pH of the solution to 4 to 5, and react for 5 to 10 minutes; 4) Use ammonia to adjust the pH of the sol to 7 to 9, and then add hexagonal Sodium phosphate, aged at 30～60°C for 0.5～2h; 5) Separate the aged mixture from solid and liquid to obtain a filter cake; 6) Dry the filter cake at 100～110°C for 1～2h, and then dry the filter cake at 300～110°C for 1～2h Baking at 400 ℃ for 1.5 to 3 hours, and cooling to obtain mesoporous silica.
Description
Technical field
The invention belongs to the resource utilization of industrial solid castoff flyash and mesopore silicon oxide synthesis technical field, tools
Body is related to a kind of method for preparing mesopore silicon oxide using flyash acid leaching residue.
Background technique
Flyash is one of the main solid waste that coal-burning power plant generates, year yield it is huge.Currently, flyash quilt
It is widely used in building materials, builds work field, utilization rate reaches 70%, and the flyash that residue is not utilized effectively is largely stored up not only
Occupy valuable land resource, and due to fugitive dust, be discharged into the modes such as water system serious influence produced on environment.
The main component of flyash is silica and aluminium oxide (60~85%), therefore the utilization of sial is powder in flyash
The important directions of coal ash.In a mild condition to flyash acidleach, then through isolating and purifying a series of available high added values
Aluminium product aluminium polychloride, metallurgical-grade aluminum oxide etc..While preparing aluminium product, silica is isolated in the form of acid leaching residue
Come.The main component of acid leaching residue is silica (> 85%), is good silicon source；But the silica in acid leaching residue cannot be answered directly
With, it is necessary to it need to be translated into sodium silicate solution, or prepare silicon materials through sodium silicate solution again.Therefore acid leaching residue efficiently prepares silicon
Acid sodium solution is the matter of utmost importance that silicon utilizes in acid leaching residue.In addition, the sodium silicate solution huge market demand, industrially passes through quartz
Sand is prepared by raw material alkali soluble under high-temperature and high-pressure conditions, and quartz sand is not only largely exploited in the technique, causes environmental disruption, and
Process energy consumption is high.Since silicon is mainly unformed silica in acid leaching residue, activity is higher, therefore alkali soluble can obtain at low temperature
Sodium silicate solution.Using the fly ash base sodium silicate solution of low cost as raw material, can further be prepared by process optimization attached
Value added higher ordered meso-porous silicon oxide material.
Mesopore silicon oxide has in fields such as catalysis, adsorbing separations and answers extensively due to having suitable specific surface area, aperture
With.It is at present largely using fly ash base sodium metasilicate for meso pore silicon oxide material as presoma using coal ash for manufacturing, in template
Auxiliary under, prepared using hydro-thermal method or sol-gel method.However, since template is expensive, silicon concentration is lower and causes to make
Higher cost, the production efficiency of standby mesopore silicon oxide are low.In addition, the sodium silicate solution of low modulus makes in material preparation process
A large amount of sodium salt is generated, post-processing is difficult, it is difficult to industrially promote and apply.It would therefore be highly desirable to develop a kind of efficient, extensive
The method for producing fly ash base mesopore silicon oxide, to meet the needs of mesopore silicon oxide is constantly grown, while also to flyash
It is sufficiently dissolved, really solves the handling problems of flyash.
In conclusion the present invention prepares the sodium silicate solution of high mode using flyash acid leaching residue as raw material, and then as
Raw material controls hydrolysis, the polymerization speed of sodium metasilicate by control chemical reaction process using simple sol-gel technology
Degree, realizes the extensive controlledly synthesis of mesopore silicon oxide, has good economy, environmental and social benefits.
Summary of the invention
The purpose of the present invention is to provide a kind of method for preparing mesopore silicon oxide using flyash acid leaching residue, this method works
Skill process is simple, low in raw material price, synthesis cost is low, synthesis process is industrially simple and easy, and energy consumption is lower.By this hair
The meso pore silicon oxide material of bright method synthesis has biggish specific surface area and Kong Rong, has broad prospects in adsorbing domain.
To achieve the above object, a kind of side that mesopore silicon oxide is prepared using flyash acid leaching residue designed by the present invention
Method, comprising the following steps:
1) flyash and sulfuric acid or hydrochloric acid solution after 100~140min of acidleach, are separated by filtration, obtain at 120~140 DEG C
Flyash acid leaching residue；
2) flyash acid leaching residue obtained in step 1) is mixed with sodium hydroxide solution according to solid-to-liquid ratio 1:2~1:4,
0.5~2h of dissolution reaction, reaction terminate, filter while hot at 60~90 DEG C, obtain soluble glass of high modulus；
3) concentration for adjusting silicon in waterglass is 20~60g/L, is 4 with the pH value that sulfuric acid adjusts high-modulus sodium silicate solution
~5,5~10min of sol gel reaction is carried out, colloidal sol is obtained；
4) with ammonium hydroxide adjust colloidal sol pH value be 7~9, add calgon, at 30~60 DEG C aging 0.5~
2h, wherein the mass ratio of calgon and waterglass is 0.05~0.2%；
5) solidliquid mixture after step 4) aging is separated by solid-liquid separation, by filtering, being washed to pH value in
Property, obtain filter cake；
6) filter cake obtained in step 5) is dried to 1~2h at 100~110 DEG C, then is roasted at 300~400 DEG C
1.5~3h obtains mesopore silicon oxide after cooling.
Preferably, the concentration of hydrochloric acid solution is 20~37% in the step 1), and the concentration of sulfuric acid solution is 20
~40%.
Preferably, the concentration of sodium hydroxide solution is 5~15% in the step 2), sodium hydroxide solution and acid
The liquid-solid ratio of phase analysis is 1:3.
Preferably, the concentration of silicon is 40~60g/L in adjustment waterglass in the step 3), the sulfuric acid
Concentration is 5~20%.
Preferably, the concentration of ammonium hydroxide is 5~25% in the step 4), and aging temperature is 40~50 DEG C, aging
Time is 1~2h；The mass ratio of the calgon and waterglass is 0.05~0.15%.
Preferably, drying temperature is 105 DEG C in the step 5), and maturing temperature is 350 DEG C.
Preferably, mesopore silicon oxide specific surface area obtained in the step 6) reaches 452m2/ g, average pore size
For 13.22nm.
The beneficial effects of the present invention are:
First, for the present invention program using industrial waste flyash acid leaching residue as raw material, reaction condition is mild, obtained waterglass
Purity is high, had not only realized the resource utilization of flyash, but also had synthesized widely used mesopore silicon oxide, realized the conjunction of resource
Reason utilizes.
Second, using high mode, the sodium silicate solution synthesizing mesoporous monox of high concentration, improve the life of mesopore silicon oxide
Efficiency is produced, the cost of post-processing is reduced.
Third, the present invention program do not add template, and the water of sodium silicate solution is controlled by the way that a small amount of calgon is added
Solution and condensation rate, have synthesized the controllable mesopore silicon oxide of pore structure, between 10~20nm, specific surface area is up to average pore size
452m2/g。
Detailed description of the invention
Fig. 1 is the process flow chart of the method for the present invention.
Fig. 2 is the nitrogen adsorption curve graph of product mesopore silicon oxide in the present invention.
Specific embodiment
Below by specific embodiment, the present invention is further illustrated, but the content of present invention is not limited only to these implementations
Example.
The flyash acid leaching residue raw material that following specific embodiments use is by by industrial waste flyash and sulfuric acid or salt
Acid solution after 100~140min of acidleach, filters, isolated flyash acid leaching residue at 120~140 DEG C.Flyash acid leaching residue
Middle composition and content are shown in Table 1；
Embodiment 1
It is that 1:2.5 is mixed according to solid-to-liquid ratio that a certain amount of acid leaching residue, which is weighed, with 10wt.% sodium hydroxide solution, at 80 DEG C
Under the conditions of dissolve 1h, reaction terminates, and filters while hot, obtains soluble glass of high modulus.Silicon concentration in waterglass is adjusted to 40g/L,
Its pH value is adjusted to 2.0 with 10wt.% sulfuric acid solution, and in normal-temperature reaction 30min；Mixed system is adjusted with 20wt.% ammonium hydroxide
PH value be 7.0,0.15% calgon is added, the aging 2h at 40 DEG C；After reaction, to solidliquid mixture into
It is capable to be separated by solid-liquid separation, isolated solid powder is dried into 1.5h, then roast 1.5h at 400 DEG C at 105 DEG C, obtained mesoporous
Silica product.
Embodiment 2
It is that 1:3 is mixed according to solid-to-liquid ratio that a certain amount of acid leaching residue, which is weighed, with 15wt.% sodium hydroxide solution, in 90 DEG C of conditions
Lower dissolution 0.5h, reaction terminate, filter while hot, obtain soluble glass of high modulus.Silicon concentration in waterglass is adjusted to 50g/L, is used
20wt.% sulfuric acid adjusts its pH value to 2.5, and in normal-temperature reaction 30min；The pH value of mixed system is adjusted with 15wt% ammonium hydroxide
It is 8.0,0.10% calgon is added, the aging 2h at 50 DEG C；After reaction, solid-liquid point is carried out to solidliquid mixture
From, by isolated solid powder at 105 DEG C dry 1h；3h is roasted at 350 DEG C again, obtains mesoporous oxidation after cooling
Silicon.
Embodiment 3
It weighs a certain amount of acid leaching residue and is mixed with 10wt.% sodium hydroxide solution according to 1:4 solid-to-liquid ratio, under the conditions of 90 DEG C
1.5h is dissolved, reaction terminates, filters while hot, obtains soluble glass of high modulus.Silicon concentration in waterglass is adjusted to 60g/L, is used
30wt.% sulfuric acid adjusts its pH value to 3.0, and in normal-temperature reaction 30min；The pH value of mixed system is adjusted with 25wt.% ammonium hydroxide
It is 9.0,0.05% calgon is added, the aging 2h at 60 DEG C；After reaction, solidliquid mixture is subjected to solid-liquid
Isolated solid powder is dried at 100 DEG C 2h, then roasts 2h at 300 DEG C by separation, obtains mesoporous oxidation after cooling
Silicon.
It is found that adsorption curve is IV type curve from the nitrogen adsorption curve graph of mesopore silicon oxide shown in Fig. 2, show oxygen
SiClx has typical meso-hole structure, and the specific surface area of gained mesopore silicon oxide reaches 452m2/ g, average pore size 13.22nm.
Table 1
Composition and content table in flyash acid leaching residue
The above described specific embodiments of the present invention are not intended to limit the scope of the present invention..Any basis
Any other various changes and modifications that technical concept of the invention is made should be included in the guarantor of the claims in the present invention
It protects in range.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811395289.6A CN109665534B (en) | 2018-11-22 | 2018-11-22 | A method for preparing mesoporous silica by using fly ash acid leaching slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811395289.6A CN109665534B (en) | 2018-11-22 | 2018-11-22 | A method for preparing mesoporous silica by using fly ash acid leaching slag |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109665534A true CN109665534A (en) | 2019-04-23 |
| CN109665534B CN109665534B (en) | 2022-05-20 |
Family
ID=66142281
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811395289.6A Active CN109665534B (en) | 2018-11-22 | 2018-11-22 | A method for preparing mesoporous silica by using fly ash acid leaching slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109665534B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110364722A (en) * | 2019-08-11 | 2019-10-22 | 山西大学 | A carbon-silicon double-shell hollow structure composite microsphere and its preparation method and application |
| CN112408401A (en) * | 2020-10-29 | 2021-02-26 | 中国建筑材料科学研究总院有限公司 | Method for preparing silicon dioxide aerogel by utilizing industrial solid waste fly ash and silicon dioxide aerogel prepared by method |
| CN116986601A (en) * | 2023-08-22 | 2023-11-03 | 西安交通大学 | Method for preparing silicon-based micro-nano material based on coal-based solid waste by micro-chemical technology |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4386057A (en) * | 1982-03-17 | 1983-05-31 | The United States Of America As Represented By The United States Department Of Energy | Recovery of iron oxide from coal fly ash |
| CN101045538A (en) * | 2007-05-08 | 2007-10-03 | 浙江大学 | Method for preparing modified silicon oxide using coal series kaolin rock or flyash |
| CN103738972A (en) * | 2013-12-27 | 2014-04-23 | 中国神华能源股份有限公司 | Method for preparing silicon micropowder by using pulverized fuel ash aluminum extraction residues |
| CN104773739A (en) * | 2015-01-14 | 2015-07-15 | 南阳东方应用化工研究所 | Fly ash decomposition method |
| CN105523558A (en) * | 2016-01-18 | 2016-04-27 | 中国地质大学（武汉） | Resource-converting comprehensive utilization process for fly ash |
| CN105776236A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Method for preparing sodium silicate by means of ordinary pulverized coal ash of pulverized coal furnace |
-
2018
- 2018-11-22 CN CN201811395289.6A patent/CN109665534B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4386057A (en) * | 1982-03-17 | 1983-05-31 | The United States Of America As Represented By The United States Department Of Energy | Recovery of iron oxide from coal fly ash |
| CN101045538A (en) * | 2007-05-08 | 2007-10-03 | 浙江大学 | Method for preparing modified silicon oxide using coal series kaolin rock or flyash |
| CN103738972A (en) * | 2013-12-27 | 2014-04-23 | 中国神华能源股份有限公司 | Method for preparing silicon micropowder by using pulverized fuel ash aluminum extraction residues |
| CN104773739A (en) * | 2015-01-14 | 2015-07-15 | 南阳东方应用化工研究所 | Fly ash decomposition method |
| CN105523558A (en) * | 2016-01-18 | 2016-04-27 | 中国地质大学（武汉） | Resource-converting comprehensive utilization process for fly ash |
| CN105776236A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Method for preparing sodium silicate by means of ordinary pulverized coal ash of pulverized coal furnace |
Non-Patent Citations (1)
| Title |
|---|
| K.S. HUI ET AL.: "Synthesis of MCM-41 from coal fly ash by a green approach: Influence of synthesis pH", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110364722A (en) * | 2019-08-11 | 2019-10-22 | 山西大学 | A carbon-silicon double-shell hollow structure composite microsphere and its preparation method and application |
| CN112408401A (en) * | 2020-10-29 | 2021-02-26 | 中国建筑材料科学研究总院有限公司 | Method for preparing silicon dioxide aerogel by utilizing industrial solid waste fly ash and silicon dioxide aerogel prepared by method |
| CN116986601A (en) * | 2023-08-22 | 2023-11-03 | 西安交通大学 | Method for preparing silicon-based micro-nano material based on coal-based solid waste by micro-chemical technology |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109665534B (en) | 2022-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103848439B (en) | Synthetic method of ZSM-5 type molecular sieve | |
| CN110040743A (en) | A kind of coal ash for manufacturing for SSZ-13 molecular sieve method | |
| CN100434364C (en) | Synthesis of Zeolite 4A by Low-temperature Alkali Fusion of Kaolin | |
| CN108059171B (en) | A kind of method for synthesizing HZSM-5 type zeolite from fly ash | |
| CN101381086B (en) | A kind of preparation method of Si-MCM-41 mesoporous molecular sieve | |
| CN106745027B (en) | A kind of method of flyash synthesis analcime | |
| CN109665534A (en) | A method of mesopore silicon oxide is prepared using flyash acid leaching residue | |
| CN109354029A (en) | A method for preparing mesoporous silica from fly ash | |
| CN104108723A (en) | Hydrothermal synthesis method of 4A molecular sieve from high-iron bauxite tailings | |
| CN104773740A (en) | Method for synchronously preparing type-A zeolite and white carbon black with fly ash | |
| CN103769045B (en) | A kind of preparation method of fly ash base high-performance adsorbing material | |
| CN101148332A (en) | A method for increasing silicon dioxide content and producing white carbon black from silica fume | |
| CN108658092B (en) | Method for preparing P-type molecular sieve and high-silicon mordenite from aluminum residue extracted by fly ash acid method and utilization method of fly ash | |
| CN103172080A (en) | Method for preparing mesoporous molecular sieve | |
| CN109336161B (en) | A kind of preparation method of CeO2 nanotube, CeO2 nanotube and application | |
| CN106495181A (en) | A kind of method that flyash synthesizes y-type zeolite | |
| CN106865565A (en) | A kind of flyash synthesizes the method for X-type zeolite | |
| CN109502679B (en) | Method for preparing flocculating agent and porous material by synergistic utilization of multiple elements of fly ash | |
| CN108726534B (en) | Preparation method of micro-mesoporous ZSM-5 molecular sieve | |
| CN107324352A (en) | A kind of method that blast furnace slag prepares ordered mesoporous silica dioxide | |
| CN105217648A (en) | Method for preparing mesoporous microporous NaY/MCM-41 composite molecular sieve by using coal gangue and silica fume as raw materials | |
| CN107298444A (en) | It is a kind of using preparation of the abietyl Gemini surface active agent as the Metaporous silicon dioxide material of template and its performance | |
| CN103073019A (en) | Hierarchical pore zeolite molecular sieve preparation method | |
| CN106111139A (en) | A kind of hydrothermal composite method of natural opal and TiO2 | |
| CN108946754A (en) | SBA-15 mesopore molecular sieve and preparation method and application and flyash produce the method for aluminium oxide and SBA-15 mesopore molecular sieve |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |