CN103710023B - Method for preparing porous photoluminescence material by utilization of rice husks - Google Patents
Method for preparing porous photoluminescence material by utilization of rice husks Download PDFInfo
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- CN103710023B CN103710023B CN201310648472.3A CN201310648472A CN103710023B CN 103710023 B CN103710023 B CN 103710023B CN 201310648472 A CN201310648472 A CN 201310648472A CN 103710023 B CN103710023 B CN 103710023B
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Abstract
The invention discloses a method for preparing a porous photoluminescence material by utilization of rice husks. In the method, pretreatment is carried out first, including that, etching is performed for 30-300min in an acidic aqueous solution with a concentration of 0.01-30wt% at the temperature of 20-300 DEG C, and after washing, drying is carried out; then thermal chemical modification is carried out, including that, the products are subjected to pyrolysis for 10-300min at the temperature of 400-1500 DEG C in vacuum and nitrogen or argon atmosphere, and a silicon carbon composite material is prepared; finally, thermal oxidation decomposition is carried out, including that, the products are subjected to combustion for 10-300min at the temperature of 400-1000 DEG C in oxygen or air atmosphere, and a porous photoluminescence material is prepared. The prepared porous photoluminescence material by utilization of rice husks as raw materials has adjustable pore sizes, has no heavy metal elements, and has high luminous intensity at the room temperature. The porous photoluminescence material has advantages of simple production technology, low cost, wide range of raw material sources, renewability and the like.
Description
Technical field
The present invention relates to a kind of hole optical electroluminescent material, be specifically related to a kind of method utilizing rice husk to prepare hole optical electroluminescent material; Belong to technical field of material chemistry.
Background technology
Embedded photoluminescent material has widespread use in illumination, information displaying, biological detection and the field such as imaging, photoelectric device.Current commercial embedded photoluminescent material needs short ultraviolet to excite usually, thus causes fluorescent lamp and electricity-saving lamp generally to adopt mercury vapour as excitaton source.Even if by European up-to-date environmental protection standard, the mercury content of an electricity-saving lamp is about 3 to 5 milligrams, once broken, the mercury of 3 milligrams will pollute the air more than 1000 tons of water or 300 cubic metres! Photoluminescent material can change long wave ultraviolet into visible ray, thus replaces the application of current mercury at fluorescent lamp and electricity-saving lamp.But the synthesis of current embedded photoluminescent material adopts the metal of the high or environmental toxic of price usually, as silver, cadmium, germanium or rare earth element etc.
In a word, there is the high and high in cost of production problem of complex process, heavy metal content in the production method of existing embedded photoluminescent material, cannot produce market in the urgent need to environmental friendliness, low cost, can be mass-produced embedded photoluminescent material.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, a kind of method utilizing rice husk to prepare embedded photoluminescent material be provided, there is environmental friendliness, technique is simple, cost is low, feature that raw material sources are wide.
China's first farm crop Year Of Rice output about 200,000,000 tons, wherein produces about 4,000 ten thousand tons, rice husk after Rice producing.Oxide compound containing the element such as a large amount of silicon-dioxide (more than 85wt%) and a small amount of potassium, calcium, iron, magnesium in ashes after combusting rice hull, as can be seen here, rice husk can as the desirable feedstock of producing silica-base material.
The present invention take rice husk as raw material, by pre-treatment and thermochemistry modified, the element beyond silicon-dioxide and carbon all can be reduced to pole low-level, then is decomposed the porous silica embedded photoluminescent material can preparing different carbon doping by thermooxidizing.
In order to achieve the above object, present invention employs following technical scheme:
Utilize rice husk to prepare a method for hole optical electroluminescent material, comprise the following steps:
(1) pre-treatment: the rice husk of 100 mass parts being added concentration is in the acidic aqueous solution of 0.01 ~ 30wt%, processes 30 minutes ~ 300 minutes under 20 ~ 300 DEG C of temperature condition, dry after washing; Described acidic solution is the combination solution that strong acid forms with hydrogen peroxide or dioxide peroxide;
(2) thermochemistry modification: by step (1) products therefrom in vacuum, nitrogen or argon gas atmosphere, and under 400 DEG C ~ 1500 DEG C temperature condition, pyrolysis 10 minutes ~ 300 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in oxygen or air atmosphere, burns and prepare hole optical electroluminescent material in 10 minutes ~ 300 minutes at 400 DEG C ~ 1000 DEG C.
For realizing the object of the invention further, in step (1), described strong acid be preferably in sulfuric acid, hydrochloric acid, nitric acid or perchloric acid one or more, the mass ratio of strong acid and hydrogen peroxide or dioxide peroxide is preferably 1:0.1 ~ 10.
In step (1), the mass ratio of described acidic solution and powdered rice hulls is preferably (5 ~ 20): 1.
In step (2), the temperature of described pyrolysis is preferably 600 DEG C ~ 900 DEG C.
In step (3), the temperature of described burning is preferably 500 DEG C ~ 700 DEG C.
Relative to prior art, tool of the present invention has the following advantages:
(1) the present invention regulates and controls pore size and pore volume by controlling pre-treatment, thermochemistry modification and thermal decomposition process, and the embedded photoluminescent material aperture of preparation is controlled.
(2) the embedded photoluminescent material composition prepared of method of the present invention is based on silicon-dioxide, heavy metal free pollution problem;
(3) method of the present invention has that production technique is simple, cost is low, raw material sources are wide, (China produces about 4,000 ten thousand tons, rice husk per year to reproducible advantage, wherein the content of silicon-dioxide is about 8,000,000 tons, therefore, rice husk can as the desirable feedstock of producing silica-base material.The present invention take rice husk as raw material, by simple pre-treatment and thermochemistry modified, below the 0.1wt.% that element beyond silicon-dioxide and carbon all can be reduced to, can prepare the porous silica embedded photoluminescent material of different carbon doping by controlling thermooxidizing decomposition course).
Accompanying drawing explanation
Fig. 1 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 1.
Fig. 2 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 2.
Fig. 3 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 3.
Fig. 4 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 4.
Fig. 5 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 5.
Fig. 6 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 6.
Fig. 7 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 7.
Fig. 8 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 8.
Fig. 9 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 9.
Figure 10 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 10.
Figure 11 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 11.
Figure 12 is the emmission spectrum of hole optical electroluminescent material prepared by the embodiment of the present invention 12.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further illustrated, but claimed scope of the present invention is not limited to the scope of embodiment statement.
Embodiment 1
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 DEG C, processes 120 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in nitrogen atmosphere, under 600 DEG C of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 120 minutes at 550 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 1) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 322m
2/ g, aperture is 5.4nm, and pore volume is 0.53cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is at 490nm.
Embodiment 2
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 0.01% hydrochloric acid and 0.1% hydrogen peroxide, at 300 DEG C, processes 30 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in argon gas atmosphere, under 1500 DEG C of temperature condition, pyrolysis 10 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 10 minutes at 1000 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 2) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 98m
2/ g, aperture is 87nm, and pore volume is 0.12cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is respectively at 450nm and 520nm.
Embodiment 3
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 30% hydrochloric acid and 5% dioxide peroxide, at 20 DEG C, processes 300 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in nitrogen atmosphere, under 400 DEG C of temperature condition, pyrolysis 300 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 300 minutes at 400 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 3) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 289m
2/ g, aperture is 6.8nm, and pore volume is 0.46cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is at 430nm.
Embodiment 4
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g containing 10% hydrochloric acid, in the 1000g aqueous solution of 1% hydrogen peroxide and 1% dioxide peroxide, at 200 DEG C, processes 120 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in nitrogen atmosphere, under 600 DEG C of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 200 minutes at 500 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 4) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 301m
2/ g, aperture is 6.1nm, and pore volume is 0.55cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is at 450nm.
Embodiment 5
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 0.5% hydrochloric acid and 0.5% hydrogen peroxide, at 150 DEG C, processes 120 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in nitrogen atmosphere, under 800 DEG C of temperature condition, pyrolysis 60 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 40 minutes at 700 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 5) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 268m
2/ g, aperture is 7.5nm, and pore volume is 0.46cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is at 590nm.
Embodiment 6
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g containing 10% hydrochloric acid, in the 1000g aqueous solution of 5% dioxide peroxide and 5% hydrogen peroxide, at 80 DEG C, processes 180 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in nitrogen atmosphere, under 500 DEG C of temperature condition, pyrolysis 240 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 40 minutes at 650 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 6) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 298m
2/ g, aperture is 6.3nm, and pore volume is 0.51cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is at 510nm.
Embodiment 7
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 DEG C, processes 120 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in nitrogen atmosphere, under 1000 DEG C of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 80 minutes at 750 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 7) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 211m
2/ g, aperture is 12nm, and pore volume is 0.33cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is at 520nm.
Embodiment 8
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 0.5% hydrochloric acid and 0.5% hydrogen peroxide, at 100 DEG C, processes 120 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in nitrogen atmosphere, under 1200 DEG C of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 120 minutes at 800 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 8) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 178m
2/ g, aperture is 28nm, and pore volume is 0.26cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is respectively at 450nm and 510nm.
Embodiment 9
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 0.1% hydrochloric acid and 0.1% hydrogen peroxide, at 100 DEG C, processes 180 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in nitrogen atmosphere, under 900 DEG C of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 90 minutes at 650 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 9) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 186m
2/ g, aperture is 17nm, and pore volume is 0.31cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is respectively at 460nm and 525nm.
Embodiment 10
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 DEG C, processes 120 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom under 600 DEG C of temperature condition, vacuum pyrolysis 120 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 150 minutes at 550 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 10) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 278m
2/ g, aperture is 5.3nm, and pore volume is 0.45cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is at 425nm.
Embodiment 11
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 DEG C, processes 120 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in argon gas atmosphere, under 600 DEG C of temperature condition, pyrolysis 180 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in oxygen, burns and prepare hole optical electroluminescent material in 90 minutes at 550 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 11) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 313m
2/ g, aperture is 4.9nm, and pore volume is 0.56cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is at 440nm.
Embodiment 12
(1) pre-treatment: by percentage to the quality, adds the rice husk of 100g in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 DEG C, processes 120 minutes, dry after washing;
(2) thermolysis: by step (1) products therefrom in nitrogen atmosphere, under 550 DEG C of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in atmosphere, burns and prepare hole optical electroluminescent material in 240 minutes at 500 DEG C.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the full-automatic specific surface area of U.S. Mike company's T riStar type and Porosimetry test material, adopt the luminescent properties (the results are shown in Figure 12) of FDAC F ?4500 type fluorescence spectrophotometer test material.The specific surface area of this sample is 276m
2/ g, aperture is 4.9nm, and pore volume is 0.52cm
3/ g, under the ultraviolet excitation of 365nm, sample presents strong luminescence, and luminous peak position is at 580nm.
Embodiment 1 ?12 test case as shown in table 1.
The specific surface area of table 1 embodiment 1 ~ 12 gained sample and pore structure
As can be seen from Table 1, the embedded photoluminescent material that prepared by the present invention has nano-porous structure.Embodiment 1 ~ 12 gained sample all has higher specific surface area and pore volume, and aperture is adjustable from 4.9nm to 87nm.The combination of vesicular structure and photoluminescence performance can widen the Application Areas of this material further, is expected in biological monitoring and imaging, administration and silicon optoelectronic be integrated etc. that field obtains applies.
As can be seen from Fig. 1 ~ 12, embedded photoluminescent material prepared by the present invention has good luminescent properties under the optical excitation of 365nm long wave ultraviolet, and luminous peak position is adjustable between 425nm ~ 580nm.
China produces about 4,000 ten thousand tons, rice husk per year, and occupy first place in the world, wherein the content of silicon-dioxide is about 8,000,000 tons, and therefore, rice husk can as the desirable feedstock of producing silica-base material.But rice husk is processed by as refuse as a rule, i.e. waste resource but also contaminate environment.The present invention take rice husk as raw material, by simple pre-treatment and thermochemistry modification and control thermooxidizing decomposition course and can prepare the adjustable silicon-dioxide embedded photoluminescent material in aperture, simultaneously the embedded photoluminescent material composition prepared of method of the present invention is based on silicon-dioxide, heavy metal free pollution problem.The invention provides the method preparing hole optical electroluminescent material with rice husk, not only solve the pollution problem of rice husk, and solve the high and problem of environmental pollution of the ubiquitous cost of current embedded photoluminescent material, and the combination of vesicular structure and photoluminescence performance can widen the Application Areas of this material further, be expected in biological monitoring and imaging, administration and silicon optoelectronic be integrated etc. that field obtains applies.
Claims (5)
1. utilize rice husk to prepare a method for hole optical electroluminescent material, it is characterized in that, comprise the following steps:
(1) pre-treatment: the rice husk of 100 mass parts being added concentration is in the acidic aqueous solution of 0.01 ~ 30wt%, processes 30 minutes ~ 300 minutes under 20 ~ 300 DEG C of temperature condition, dry after washing; Described acidic solution is the combination solution that strong acid forms with hydrogen peroxide or dioxide peroxide;
(2) thermochemistry modification: by step (1) products therefrom in vacuum, nitrogen or argon gas atmosphere, and under 400 DEG C ~ 1500 DEG C temperature condition, pyrolysis 10 minutes ~ 300 minutes, prepares Si-C composite material;
(3) thermooxidizing is decomposed: by step (2) products therefrom in oxygen or air atmosphere, burns and prepare hole optical electroluminescent material in 10 minutes ~ 300 minutes at 400 DEG C ~ 1000 DEG C.
2. method according to claim 1, is characterized in that, in step (1), described strong acid is one or more in sulfuric acid, hydrochloric acid, nitric acid or perchloric acid, and the mass ratio of strong acid and hydrogen peroxide or dioxide peroxide is 1:0.1 ~ 10.
3. method according to claim 2, is characterized in that, in step (1), the mass ratio of described acidic solution and rice husk is (5 ~ 20): 1.
4. method according to claim 2, is characterized in that, in step (2), the temperature of described pyrolysis is 600 DEG C ~ 900 DEG C.
5. method according to claim 2, is characterized in that, in step (3), the temperature of described burning is 500 DEG C ~ 700 DEG C.
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| CN1202993C (en) * | 2003-05-20 | 2005-05-25 | 吉林大学 | Process for preparing high-purity nano silicon dioxide from rice husk |
| CN1935648B (en) * | 2006-09-14 | 2010-05-12 | 华南理工大学 | Method for preparing polycrystalline silicon for solarcell from rice husk |
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| CN101920966B (en) * | 2010-07-21 | 2012-07-04 | 化工部长沙设计研究院 | Method for producing porous nano silica and active carbon by utilizing rice hull ash |
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