CN1117029C - Preparation of nanometer SiO2 pipe and nanometer Al2O3 crystal - Google Patents
Preparation of nanometer SiO2 pipe and nanometer Al2O3 crystal Download PDFInfo
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- CN1117029C CN1117029C CN01119430A CN01119430A CN1117029C CN 1117029 C CN1117029 C CN 1117029C CN 01119430 A CN01119430 A CN 01119430A CN 01119430 A CN01119430 A CN 01119430A CN 1117029 C CN1117029 C CN 1117029C
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- kaolin
- nanometer
- pipe
- nanometer pipe
- silica nanometer
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a method for preparing silicon dioxide nanotubes and aluminum oxide nanocrystals from kaolin as raw materials, which comprehensively utilizes various useful elements to prepare Silicon dioxide nanotubes, aluminum oxide nanocrystals and sodium sulfate or sodium chloride. Products prepared with the method are widely used in the technical field of rubber, plastics, paint, printing ink, papermaking, building material, daily chemicals, etc. Especially used as reinforcing agents of rubber and plastic products, the silicon dioxide nanotubes can compete with any low-grade reinforcing agent in prices, can compete with any high-grade reinforcing agent in performance, and have the advantages of simple production process, cheap and rich raw materials and excellent performance.
Description
The present invention relates to nanocrystalline and preparation method nanotube, particularly relating to a kind of is the method for feedstock production silica nanometer pipe with kaolin.
China is the country of kaolin reserves maximum, and ground reserves such as (Huijiang, pear tree), Sichuan are particularly abundant especially in Jilin.Present domestic kaolin is mainly used in as general filler, and of poor quality because of product specification is low, added value is low, and reasons such as the wasting of resources have seriously limited the Application Areas of product, to such an extent as to economic benefit is not very good.Utilize new technology that low value-added common kaolin is prepared into high value-added product and not only can make this conventional industries search out road for development, and be the important topic of comprehensive utilization natural resource.
What purpose of the present invention just provided that a kind of technology is simple, easy to operate, cost is low, added value is high is the method for feedstock production silica nanometer pipe with kaolin.
The present invention at first carries out thaumatropy with the kaolin roasting, and maturing temperature is 600～1000 ℃, and the time is 10～24 hours, grind be 1～15 μ m after, with kaolin powder and concentration is that 20%～80% acidic solution mixes by 1: 2～8 (weight), is 80～160 ℃ in temperature and reacts 2～20 hours down, filters, filter cake is through being washed to neutrality, drying gets tubular nanometer silicon-dioxide, and internal diameter is 20～40nm, external diameter is 90-100nm, and length-to-diameter ratio is 5～10.Filtrate adds alkali (as NaOH, NH
3H
2O) neutralize aluminum hydroxide precipitation, filter, filter cake is through being washed to neutrality, through 200-600 ℃ of roasting 6-12 hour diameter be the aluminium sesquioxide nano crystal material of 20～80nm, concentrating filter liquor gets sodium salt, is sodium sulfate or sodium-chlor or SODIUMNITRATE.
The employed acidic substance of said process are H
2SO
4, HCl, HNO
3, wherein with H
2SO
4Be the best.
The silica nanometer pipe has the special property that is different from general silica, and incomparable advantage is arranged.The heat of silica nanometer pipe, magnetic, light, sensitivity characteristic and stability all are different from common silicon-dioxide, also have as high reactivity, high epistasis, high rigidity and good advantages such as plasticity, not only the uv reflectance ability is strong, good stability, and low Young's modulus, thermal conductivity and good absorption property etc. also make the silica nanometer pipe have good application prospects in fields such as rubber, plastics, coating, printing ink, papermaking, building materials, daily use chemicals.
Be the various elements that contained in the comprehensive utilization kaolin, when utilizing element silicon to prepare the silica nanometer pipe of excellent property, utilize aluminium element to prepare nano-aluminium oxide, and utilize raffinate to synthesize sodium sulfate, thereby fully improved kaolinic comprehensive utilization ratio.Nano-aluminium oxide can be widely used in producing high technology ceramics material, fluorescent material, wet electrical material as a kind of important chemical material, on chemical industry, can be used as the purifying of strainer, separator, high-purity gas etc.Sodium sulfate further reduces the cost of product as byproduct, and can be enterprise increases considerable economic, strengthens Enterprises'Competitiveness.
Because the singularity of silica nanometer tube shape structure, have incomparable advantage than hard(carbon)black, white carbon black as the reinforced filling of rubber, plastics:
1. big fineness ratio will make reinforcing property increase substantially;
With recombination processes such as rubber, plastics in, polymer can enter in the pipe of nano material, produces special bonding force, and reinforcing property is increased substantially;
3. because the wear resistance of silicon-dioxide itself and the reinforcement of tubular structure, the silica nanometer pipe can be applied in the high-grade rubber item (as tire etc.), improve the intensity index and the wear-resistant index of present tire, may bring revolutionary variation to homemade tire after studying successfully, participate in competition in the international market.
4. the high high-temp stability of silicon-dioxide and erosion resistance make its strengthening agent as high-grade goods have peculiar advantage, are that other nano material fillers are incomparable;
5. silica product is in the market competition process, and worst factor is that production cost is than other mineral filler height.And utilize kaolin to prepare the silica nanometer pipe, and again kaolin is fully utilized, the preparation cost of silica nanometer pipe is reduced significantly, production cost is lower than any high and low shelves reinforcement product.
In a word, the silica nanometer pipe can be competed with any strengthening agent of keeping out on price, can compete with any high-grade strengthening agent on performance.
In sum, with kaolin be raw material production prepare the silica nanometer pipe and aluminium sesquioxide nanocrystalline, not only production technique is simple, low price, excellent performance, and have a series of important development and application values, advantage such as industrialization prospect is good.
Below in conjunction with embodiment the present invention is further described:
Embodiment 1: maturing temperature is 700 ℃, and the time is 13 hours, and grinding is 6 μ m.With the kaolin after the roasting pulverizing 1 part of (weight) and 2 part of 50% H
2SO
4Mixing was reacted 4 hours down at 130 ℃, and cooling is filtered, and filter cake is through being washed to neutrality, and drying gets tubular nanometer silicon-dioxide, and mean inside diameter is 30nm, and external diameter is 95nm, and length-to-diameter ratio is 7.Filtrate add NaOH solution neutralize aluminum hydroxide precipitation, filter, filter cake is through being washed to neutrality, through 300 ℃ of roastings 8 hours mean diameter be the aluminium sesquioxide nano crystal material of 50nm, concentrating filter liquor gets sodium sulfate.
Embodiment 2: maturing temperature is 850 ℃, and the time is 18 hours, and grinding is 11 μ m.Kaolin 1 part (weight) after the roasting pulverizing is mixed with 3 part of 40% HCl, reacted 4 hours down at 130 ℃, cooling is filtered, and filter cake is through being washed to neutrality, and drying gets tubular nanometer silicon-dioxide, and mean inside diameter is 35nm, and external diameter is 102nm, and length-to-diameter ratio is 6.5.Filtrate add NaOH solution neutralize aluminum hydroxide precipitation, filter, filter cake is through being washed to neutrality, through 350 ℃ of roastings 9 hours mean diameter be the aluminium sesquioxide nano crystal material of 40nm, concentrating filter liquor gets sodium-chlor.
Embodiment 3: maturing temperature is 800 ℃, and the time is 14 hours, and grinding is 13 μ m.With the kaolin after the roasting pulverizing 1 part of (weight) and 5 part of 40% HNO
3Mixing was reacted 6 hours down at 100 ℃, and cooling is filtered, and filter cake is through being washed to neutrality, and drying gets tubular nanometer silicon-dioxide, and mean inside diameter is 32nm, and external diameter is 130nm, and length-to-diameter ratio is 6.Filtrate add NaOH solution neutralize aluminum hydroxide precipitation, filter, filter cake is through being washed to neutrality, through 450 ℃ of roastings 9 hours mean diameter be the aluminium sesquioxide nano crystal material of 42nm, concentrating filter liquor gets SODIUMNITRATE.
Claims (4)
1, a kind of is the method for feedstock production silica nanometer pipe with kaolin, it is characterized in that:
A: at first kaolin is carried out roasting, maturing temperature is 600-1000 ℃, and the time is 10-
24 hours;
B: kaolin grinds the m into 1-15 μ after the roasting, is 20%-with kaolin powder and concentration
80% acidic solution is by 1: 2-8 (weight) mixes, and is anti-under temperature is 80-160 ℃
Answered 2-20 hour, and filtered, filter cake is through being washed to neutrality, and drying must bore be 20
-40nm, external diameter are 90-100nm, and length-to-diameter ratio is the tubular nanometer silicon-dioxide of 5-10.
2, described as right 1 is the method for feedstock production silica nanometer pipe with kaolin, its feature
Be that described acidic substance are H
2SO
4, HCl or HNO
3In a kind of.
3, described as right 1 is the method for feedstock production silica nanometer pipe with kaolin, its feature
Be that described acidic substance are H
2SO
4
4, described as right 1 is the method for feedstock production silica nanometer pipe with kaolin, its feature
Be that described alkali is NaOH or NH
3H
2O.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01119430A CN1117029C (en) | 2001-05-25 | 2001-05-25 | Preparation of nanometer SiO2 pipe and nanometer Al2O3 crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01119430A CN1117029C (en) | 2001-05-25 | 2001-05-25 | Preparation of nanometer SiO2 pipe and nanometer Al2O3 crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1318513A CN1318513A (en) | 2001-10-24 |
| CN1117029C true CN1117029C (en) | 2003-08-06 |
Family
ID=4663649
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN01119430A Expired - Fee Related CN1117029C (en) | 2001-05-25 | 2001-05-25 | Preparation of nanometer SiO2 pipe and nanometer Al2O3 crystal |
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| CN (1) | CN1117029C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100377997C (en) * | 2006-05-21 | 2008-04-02 | 戴福寿 | Method for extracting nano silicon dioxide from calcium-base bentonite |
| CN100537854C (en) * | 2007-04-03 | 2009-09-09 | 中国科学院理化技术研究所 | A kind of preparation method of silica nanometer pipe |
| CN101112990B (en) * | 2007-07-05 | 2010-09-08 | 东北大学 | Method for co-production of white carbon black, aluminum oxide and kerogen by kerosene shale |
| CN102275938A (en) * | 2011-07-21 | 2011-12-14 | 中国地质大学（武汉） | Method for preparing silicon dioxide nanotubes from halloysite used as raw material |
| CN104556074B (en) * | 2015-01-21 | 2016-06-08 | 海南大学 | One quickly prepares uniform SiO with meerschaum for raw material2The preparation method of nanotube |
| CN108199030B (en) * | 2018-01-11 | 2020-11-03 | 南开大学 | Preparation method of porous silicon/graphite/carbon composite negative electrode material of lithium ion secondary battery |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1117022A (en) * | 1995-03-14 | 1996-02-21 | 中国科学院固体物理研究所 | Prepn of silicon dioxide powder with controllable nanon size |
| CN1183379A (en) * | 1997-12-30 | 1998-06-03 | 中国科学院感光化学研究所 | Process for preparing nm silicon dioxide granule from alkali metal silicate |
-
2001
- 2001-05-25 CN CN01119430A patent/CN1117029C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1117022A (en) * | 1995-03-14 | 1996-02-21 | 中国科学院固体物理研究所 | Prepn of silicon dioxide powder with controllable nanon size |
| CN1183379A (en) * | 1997-12-30 | 1998-06-03 | 中国科学院感光化学研究所 | Process for preparing nm silicon dioxide granule from alkali metal silicate |
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|---|---|
| CN1318513A (en) | 2001-10-24 |
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