CN104909383A - New method for synthesizing multilayer high specific surface area SBA-15 mesoporous molecular sieve - Google Patents
New method for synthesizing multilayer high specific surface area SBA-15 mesoporous molecular sieve Download PDFInfo
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- CN104909383A CN104909383A CN201510341825.4A CN201510341825A CN104909383A CN 104909383 A CN104909383 A CN 104909383A CN 201510341825 A CN201510341825 A CN 201510341825A CN 104909383 A CN104909383 A CN 104909383A
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Abstract
The invention provides a new method for synthesizing a multilayer high specific surface area SBA-15 mesoporous molecular sieve. The new method is characterized by comprising the following steps: (1) by taking rice husk ash as the raw material, preparing water glass having the modulus of greater than 5 by use of an alkaline reaction method; (2) dissolving polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer-P123 in HCl having the concentration of 2.5mol/L in the ratio of (1-3)g of P123/30ml of HCl; and after dissolving, adding the water glass, wherein the mass ratio of added water glass to P123 is 5: 8; stirring for 24 hours; then, putting the mixture into a polytetrafluoroethylene lined stainless reaction kettle and crystallizing at 100-120 DEG C for 48-72 hours; filtering and drying; and roasting at 550 DEG C for 6 hours to obtain the regular multilayer SBA-15 mesoporous molecular sieve having the specific surface area of 1000m<2>/g or above; the multilayer high specific surface are SBA-15 mesoporous molecular sieve can be applied to the fields of adsorption, separation, catalysts, catalyst supports, petrochemical industry and the like.
Description
Technical field
The invention provides a kind of novel method of synthesizing multilayer shape high-ratio surface SBA-15 mesopore molecular sieve, belong to technical field of inorganic nonmetallic materials.
Background technology
Molecular sieve has good catalytic performance, absorption property and ion exchangeable, is widely used in fields such as washing composition, petrochemical industry, medicine and environmental protection.SBA-15 is a kind of mesoporous nano material, has excellent ion-exchange, catalysis and absorption property, and in many fields such as fine chemical industry petrochemical industry, medical and health and environment protection, tool has been widely used and huge application potential.SBA-15 mesopore molecular sieve purity high-performance prepared by Conventional cryogenic hydro-thermal synthesis process is good, but its raw materials is the industrial chemicals such as tetraethoxy, water glass, higher and the limited source of price, cause preparation cost to remain high, seriously constrain the extensive use of SBA-15 mesopore molecular sieve and widening further of Application Areas.Therefore, countries in the world are devoted to find the cheap and natural aluminosilicate raw mineral materials of wide material sources, as SBA-15 mesopore molecular sieve prepared by the alternative industrial chemicals such as kaolin, perlite, foam, potassium felspar sand and natural parastilbite.
China is Rice Cropping big country, produces paddy per year 200,000,000
tabove, rice husk more than 4,000 ten thousand can be obtained after processing
t, rice husk not easily absorbs water, and being directly applied to field, to make fertilizer not perishable again.Present stage as primary fuel burning, makes a low multiple use mostly.In rice husk, main component is hydrocarbon polymer, the amorphous hydrated silica in addition containing 15 ~ 18 %, containing the Volcanic-type high reactivity silicon-dioxide of more than 90% in the rice hull ash after burning.Therefore the comprehensive utilization of rice husk is significant, and this can not only solve the pollution problem of a large amount of agricultural by-products, and can also make full use of resource.The exploitation of current rice husk silicon to extract SiO from rice husk
2be main.The present invention utilizes rice husk silicon to prepare the SBA-15 mesopore molecular sieve of high-specific surface area.
Summary of the invention
The object of the invention is to propose a kind ofly to utilize agricultural wastes rice husk to be raw material, the preparation method of the SBA-15 mesopore molecular sieve that easy and simple to handle, cost is low, product performance are excellent.Its technology contents is:
The novel method of synthesizing multilayer shape high-ratio surface SBA-15 mesopore molecular sieve, is characterized in that adopting following steps: (1) take rice hull ash as raw material, adopts alkali reaction legal system to be greater than the water glass of 5 for modulus; (2) polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer-P123 being dissolved in concentration with the ratio of (1 ~ 3) g P123/30 ml HCl is in the HCl of 2.5 mol/L, adding after dissolving with the mass ratio of P123 is the water glass of 5:8, stirring 24 h is placed in teflon-lined stainless steel cauldron, crystallization 48 ~ 72 h at 100 ~ 120 DEG C, after filtration drying, at 550 DEG C, roasting 6 h obtains the multi-lamellar specific surface area of rule up to 1000 m
2the SBA-15 mesopore molecular sieve of/more than g.
The novel method of the synthesizing multilayer shape high-ratio surface SBA-15 mesopore molecular sieve as described in claim 1, be characterised in that: be raw material with rice hull ash in step (1), adopt alkali reaction legal system for modulus be greater than 5 water glass, concrete steps are under water bath condition, be that 2 mol/L NaOH mix with (5 ~ 6) g/12 ml ratio by the rice hull ash of calcining 6 h at 550 DEG C with concentration, stirring reaction 3 ~ 5 h at 90 DEG C, obtains the water glass that modulus is more than 5.
Compared with prior art, its advantage is in the present invention:
1, utilize rice hull ash for silicon source, replace the Organic Chemicals such as tetraethoxy, cost-saving and turn waste into wealth.
2, prepared SBA-15 mesopore molecular sieve has regular many laminate structures, and specific surface area can reach 1000 m
2/ more than g.
accompanying drawing explanation:
Fig. 1 is the XRD figure of SBA-15 mesopore molecular sieve;
Fig. 2 is the SEM figure of SBA-15 mesopore molecular sieve.
Embodiment
Embodiment one:
1, the preparation of water glass: under water bath condition, be that 2 mol/ L NaOH mix with 5 g/12 ml ratios by the rice hull ash of calcining 6 h at 550 DEG C with concentration, stirring reaction 3 h at 90 DEG C, obtains the water glass that modulus is about 5.
2, the preparation of SBA-15 mesopore molecular sieve: it is in the HCl of 2.5 mol/L that polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer-P123 is dissolved in concentration with the ratio of 1g P123/30 ml HCl, adding after dissolving with the mass ratio of P123 is the water glass of 5:8, stirring 24 h is placed in teflon-lined stainless steel cauldron, crystallization 72 h at 100 DEG C, after filtration drying, at 550 DEG C, roasting 6 h obtains the multi-lamellar specific surface area of rule up to 1200 m
2the SBA-15 mesopore molecular sieve of/more than g.
Embodiment two:
1, the preparation of water glass: under water bath condition, be that 2 mol/L NaOH mix with 5.5 g/12 ml ratios by the rice hull ash of calcining 6 h at 550 DEG C with concentration, stirring reaction 4 h at 90 DEG C, obtains the water glass that modulus is about 5.
2, the preparation of SBA-15 mesopore molecular sieve: it is in the HCl of 2.5 mol/L that polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer-P123 is dissolved in concentration with the ratio of 2 g P123/30 ml HCl, adding after dissolving with the mass ratio of P123 is the water glass of 5:8, stirring 24 h is placed in teflon-lined stainless steel cauldron, crystallization 56 h at 110 DEG C, after filtration drying, at 550 DEG C, roasting 6 h obtains the multi-lamellar specific surface area of rule up to 1200 m
2the SBA-15 mesopore molecular sieve of/more than g.
Embodiment three:
1, the preparation of water glass: under water bath condition, be that 2 mol/L NaOH mix with 6 g/12 ml ratios by the rice hull ash of calcining 6 h at 550 DEG C with concentration, stirring reaction 5 h at 90 DEG C, obtains the water glass that modulus is about 5.
3, the preparation of SBA-15 mesopore molecular sieve: be dissolved in the HCl that concentration is 2.5mol/L with the ratio of 3 g P123/30 ml HCl by polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer-P123, adding with the mass ratio of P123 after dissolving completely is the SiO of 5:8
2, stir 24 h and be placed in teflon-lined stainless steel cauldron, crystallization 48 h at 120 DEG C, filtration drying is placed on roasting 6 h in the retort furnace of 550 DEG C and namely obtains SBA-15 mesopore molecular sieve.
Claims (2)
1. the novel method of synthesizing multilayer shape high-ratio surface SBA-15 mesopore molecular sieve, is characterized in that adopting following steps: (1) take rice hull ash as raw material, adopts alkali reaction legal system to be greater than the water glass of 5 for modulus; (2) polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer-P123 being dissolved in concentration with the ratio of (1 ~ 3) g P123/30 ml HCl is in the HCl of 2.5 mol/L, adding after dissolving with the mass ratio of P123 is the water glass of 5:8, stirring 24 h is placed in teflon-lined stainless steel cauldron, crystallization 48 ~ 72 h at 100 ~ 120 DEG C, after filtration drying, at 550 DEG C, roasting 6 h obtains the multi-lamellar specific surface area of rule up to 1000 m
2the SBA-15 mesopore molecular sieve of/more than g.
2. the novel method of the synthesizing multilayer shape high-ratio surface SBA-15 mesopore molecular sieve as described in claim 1, be characterised in that: step (1) take rice hull ash as raw material, alkali reaction legal system is adopted to be greater than the water glass of 5 for modulus, concrete steps are under water bath condition, be that 2 mol/L NaOH mix with (5 ~ 6) g/12 ml ratio by the rice hull ash of calcining 6 h at 550 DEG C with concentration, stirring reaction 3 ~ 5 h at 90 DEG C, obtains the water glass that modulus is more than 5.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105344337A (en) * | 2015-12-08 | 2016-02-24 | 无锡拓能自动化科技有限公司 | Preparation method for heavy metal wastewater adsorbent |
| CN106082257A (en) * | 2016-06-08 | 2016-11-09 | 清华大学 | A kind of hollow molecular sieve, preparation method and applications |
| CN106957059A (en) * | 2017-03-15 | 2017-07-18 | 西南科技大学 | A kind of method of the orderly spherical mesoporous material of controlledly synthesis |
| CN108928829A (en) * | 2017-05-24 | 2018-12-04 | 神华集团有限责任公司 | SBA-15 mesopore molecular sieve and its preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014125309A2 (en) * | 2013-02-18 | 2014-08-21 | Teesside University | Supported metal catalyst |
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2015
- 2015-06-19 CN CN201510341825.4A patent/CN104909383B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014125309A2 (en) * | 2013-02-18 | 2014-08-21 | Teesside University | Supported metal catalyst |
Non-Patent Citations (5)
| Title |
|---|
| M.CHAREONPANICH ET AL;: "Short-period synthesis of ordered mesoporous silica SBA-15 using ultrasonic technique", 《MATERIALS LETTERS》 * |
| MARGANDAN BHAGIYALAKSHMI ET AL;: "Utilization of rice husk ash as silica source for the synthesis of mesoporous silicas and their application to CO2 adsorption through TREN/TEPA grafting", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
| 刘娟等: "稻壳灰制水玻璃的正交试验研究", 《粮食与饲料工业》 * |
| 肖凯明: "稻壳灰制备有序介孔氧化硅及吸附性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 陈正行等: "稻壳基高度有序介孔二氧化硅材料的制备", 《粮食与食品工业》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105344337A (en) * | 2015-12-08 | 2016-02-24 | 无锡拓能自动化科技有限公司 | Preparation method for heavy metal wastewater adsorbent |
| CN106082257A (en) * | 2016-06-08 | 2016-11-09 | 清华大学 | A kind of hollow molecular sieve, preparation method and applications |
| CN106957059A (en) * | 2017-03-15 | 2017-07-18 | 西南科技大学 | A kind of method of the orderly spherical mesoporous material of controlledly synthesis |
| CN106957059B (en) * | 2017-03-15 | 2019-03-19 | 西南科技大学 | A kind of method of the orderly spherical mesoporous material of controlledly synthesis |
| CN108928829A (en) * | 2017-05-24 | 2018-12-04 | 神华集团有限责任公司 | SBA-15 mesopore molecular sieve and its preparation method and application |
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