CN103710023A - 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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- CN103710023A CN103710023A CN201310648472.3A CN201310648472A CN103710023A CN 103710023 A CN103710023 A CN 103710023A CN 201310648472 A CN201310648472 A CN 201310648472A CN 103710023 A CN103710023 A CN 103710023A
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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 of utilizing rice husk to prepare hole optical electroluminescent material; Belong to materials chemistry field.
Background technology
Embedded photoluminescent material has widespread use in fields such as illumination, information demonstration, biological detection and imaging, photoelectric devices.Current commercial embedded photoluminescent material needs short ultraviolet ray to excite conventionally, thereby 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 that surpasses 1000 tons of water or 300 cubic metres! Photoluminescent material can be changed long wave ultraviolet into visible ray, thereby replaces current mercury in the application of fluorescent lamp and electricity-saving lamp.But synthesizing of embedded photoluminescent material adopts the metal that price is high or environment is poisonous conventionally at present, as silver, cadmium, germanium or rare earth element etc.
In a word, there is complex process in the production method of existing embedded photoluminescent material, heavy metal content is high and high in cost of production problem, cannot produce market in the urgent need to environmental friendliness, low cost, embedded photoluminescent material can be mass-produced.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art, a kind of method of utilizing rice husk to prepare embedded photoluminescent material is provided, there is environmental friendliness, the feature that technique is simple, cost is low, raw material sources are wide.
Approximately 200,000,000 tons of the first farm crop Year Of Rice output of China, wherein produce approximately 4,000 ten thousand tons, rice husk after rice processing.The oxide compound that contains the elements 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 be used as the desirable feedstock of producing silica-base material.
The present invention be take rice husk as raw material, and after pre-treatment and thermochemistry modification, the element beyond silicon-dioxide and carbon all can be reduced to extremely low-level, then decomposes by thermooxidizing the porous silica embedded photoluminescent material that can prepare different carbon doping.
In order to achieve the above object, the present invention has adopted following technical scheme:
Utilize rice husk to prepare a method for hole optical electroluminescent material, comprise the following steps:
(1) pre-treatment: it is in the acidic aqueous solution of 0.01～30wt% that the rice husk of 100 mass parts is added to concentration is processed 30 minutes～300 minutes under 20～300 ℃ of temperature condition, dry after washing; The described acidic solution combination solution that to be strong acid form with hydrogen peroxide or dioxide peroxide;
(2) thermochemistry modification: in vacuum, nitrogen or argon gas atmosphere, and under 400 ℃～1500 ℃ temperature condition, pyrolysis 10 minutes～300 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in oxygen or air atmosphere, is burned and within 10 minutes～300 minutes, prepares hole optical electroluminescent material at 400 ℃～1000 ℃.
For further realizing the object of the invention, in step (1), described strong acid is preferably 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 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 ℃～900 ℃.
In step (3), the temperature of described burning is preferably 500 ℃～700 ℃.
With respect 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 that prepared by method of the present invention be take silicon-dioxide as main, 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 approximately 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 be used as the desirable feedstock of producing silica-base material.The present invention be take rice husk as raw material, after simple pre-treatment and thermochemistry modification, below the 0.1wt.% that element beyond silicon-dioxide and carbon all can be reduced to, by controlling thermooxidizing decomposition course, can prepare the porous silica embedded photoluminescent material of different carbon doping).
Accompanying drawing explanation
Fig. 1 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 1 preparation.
Fig. 2 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 2 preparations.
Fig. 3 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 3 preparations.
Fig. 4 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 4 preparations.
Fig. 5 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 5 preparations.
Fig. 6 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 6 preparations.
Fig. 7 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 7 preparations.
Fig. 8 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 8 preparations.
Fig. 9 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 9 preparations.
Figure 10 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 10 preparations.
Figure 11 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 11 preparations.
Figure 12 is the emmission spectrum of the hole optical electroluminescent material of the embodiment of the present invention 12 preparations.
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, the rice husk of 100g is added in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 ℃, process 120 minutes, dry after washing;
(2) thermolysis: in nitrogen atmosphere, under 600 ℃ of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 550 ℃ and within 120 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 1) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 322m
2/ g, aperture is 5.4nm, pore volume is 0.53cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is at 490nm.
Embodiment 2
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added in the 1000g aqueous solution containing 0.01% hydrochloric acid and 0.1% hydrogen peroxide, at 300 ℃, process 30 minutes, dry after washing;
(2) thermolysis: in argon gas atmosphere, under 1500 ℃ of temperature condition, pyrolysis 10 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 1000 ℃ and within 10 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 2) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 98m
2/ g, aperture is 87nm, pore volume is 0.12cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is respectively at 450nm and 520nm.
Embodiment 3
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added in the 1000g aqueous solution containing 30% hydrochloric acid and 5% dioxide peroxide, at 20 ℃, process 300 minutes, dry after washing;
(2) thermolysis: in nitrogen atmosphere, under 400 ℃ of temperature condition, pyrolysis 300 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 400 ℃ and within 300 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 3) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 289m
2/ g, aperture is 6.8nm, pore volume is 0.46cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is at 430nm.
Embodiment 4
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added containing 10% hydrochloric acid, in the 1000g aqueous solution of 1% hydrogen peroxide and 1% dioxide peroxide, at 200 ℃, process 120 minutes, dry after washing;
(2) thermolysis: in nitrogen atmosphere, under 600 ℃ of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 500 ℃ and within 200 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 4) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 301m
2/ g, aperture is 6.1nm, pore volume is 0.55cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is at 450nm.
Embodiment 5
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added in the 1000g aqueous solution containing 0.5% hydrochloric acid and 0.5% hydrogen peroxide, at 150 ℃, process 120 minutes, dry after washing;
(2) thermolysis: in nitrogen atmosphere, under 800 ℃ of temperature condition, pyrolysis 60 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 700 ℃ and within 40 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 5) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 268m
2/ g, aperture is 7.5nm, pore volume is 0.46cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is at 590nm.
Embodiment 6
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added containing 10% hydrochloric acid, in the 1000g aqueous solution of 5% dioxide peroxide and 5% hydrogen peroxide, at 80 ℃, process 180 minutes, dry after washing;
(2) thermolysis: in nitrogen atmosphere, under 500 ℃ of temperature condition, pyrolysis 240 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 650 ℃ and within 40 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 6) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 298m
2/ g, aperture is 6.3nm, pore volume is 0.51cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is at 510nm.
Embodiment 7
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 ℃, process 120 minutes, dry after washing;
(2) thermolysis: in nitrogen atmosphere, under 1000 ℃ of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 750 ℃ and within 80 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 7) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 211m
2/ g, aperture is 12nm, pore volume is 0.33cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is at 520nm.
Embodiment 8
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added in the 1000g aqueous solution containing 0.5% hydrochloric acid and 0.5% hydrogen peroxide, at 100 ℃, process 120 minutes, dry after washing;
(2) thermolysis: in nitrogen atmosphere, under 1200 ℃ of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 800 ℃ and within 120 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 8) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 178m
2/ g, aperture is 28nm, pore volume is 0.26cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is respectively at 450nm and 510nm.
Embodiment 9
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added in the 1000g aqueous solution containing 0.1% hydrochloric acid and 0.1% hydrogen peroxide, at 100 ℃, process 180 minutes, dry after washing;
(2) thermolysis: in nitrogen atmosphere, under 900 ℃ of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 650 ℃ and within 90 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 9) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 186m
2/ g, aperture is 17nm, pore volume is 0.31cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is respectively at 460nm and 525nm.
Embodiment 10
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 ℃, process 120 minutes, dry after washing;
(2) thermolysis: under 600 ℃ of temperature condition, vacuum pyrolysis 120 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 550 ℃ and within 150 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 10) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 278m
2/ g, aperture is 5.3nm, pore volume is 0.45cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is at 425nm.
Embodiment 11
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 ℃, process 120 minutes, dry after washing;
(2) thermolysis: in argon gas atmosphere, under 600 ℃ of temperature condition, pyrolysis 180 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in oxygen, is burned at 550 ℃ and within 90 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 11) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 313m
2/ g, aperture is 4.9nm, pore volume is 0.56cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is at 440nm.
Embodiment 12
(1) pre-treatment: by percentage to the quality, the rice husk of 100g is added in the 1000g aqueous solution containing 0.2% hydrochloric acid and 0.1% hydrogen peroxide, at 100 ℃, process 120 minutes, dry after washing;
(2) thermolysis: in nitrogen atmosphere, under 550 ℃ of temperature condition, pyrolysis 120 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in air, is burned at 500 ℃ and within 240 minutes, prepares hole optical electroluminescent material.
Adopt specific surface area and the pore structure (the results are shown in Table 1) of the U.S. Mike company's T full-automatic specific surface area of riStar type and pore analysis instrument test material, adopt the luminescent properties (the results are shown in Figure 12) of FDAC F ?4500 type fluorescence spectrophotometer test materials.The specific surface area of this sample is 276m
2/ g, aperture is 4.9nm, pore volume is 0.52cm
3/ g, under the ultraviolet excitation of 365nm, sample presents luminous by force, and luminous peak position is at 580nm.
Embodiment 1 ?12 test case as shown in table 1.
Specific surface area and the pore structure of table 1 embodiment 1～12 gained sample
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 Application Areas of this material can be further widened in the combination of vesicular structure and photoluminescence performance, is expected in biological monitoring and imaging, administration and silicon optoelectronic be integrated etc. that field obtains application.
By Fig. 1～12, can be found out, embedded photoluminescent material prepared by the present invention has good luminescent properties under 365nm long wave ultraviolet light excites, and luminous peak position is adjustable between 425nm～580nm.
China produces approximately 4,000 ten thousand tons, rice husk per year, occupies first place in the world, and wherein the content of silicon-dioxide is about 8,000,000 tons, and therefore, rice husk can be used as the desirable feedstock of producing silica-base material.But rice husk is used as refuse and processes as a rule, wastes resource contaminate environment again.The present invention be 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, the embedded photoluminescent material composition that simultaneously prepared by method of the present invention be take silicon-dioxide as main, heavy metal free pollution problem.The invention provides the method for preparing hole optical electroluminescent material with rice husk, not only solved the pollution problem of rice husk, and solved the high and problem of environmental pollution of the ubiquitous cost of current embedded photoluminescent material, and the Application Areas of this material can be further widened in the combination of vesicular structure and photoluminescence performance, be expected in biological monitoring and imaging, administration and silicon optoelectronic be integrated etc. that field obtains application.
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: it is in the acidic aqueous solution of 0.01～30wt% that the rice husk of 100 mass parts is added to concentration is processed 30 minutes～300 minutes under 20～300 ℃ of temperature condition, dry after washing; The described acidic solution combination solution that to be strong acid form with hydrogen peroxide or dioxide peroxide;
(2) thermochemistry modification: in vacuum, nitrogen or argon gas atmosphere, and under 400 ℃～1500 ℃ temperature condition, pyrolysis 10 minutes～300 minutes, prepares Si-C composite material by step (1) products therefrom;
(3) thermooxidizing is decomposed: step (2) products therefrom, in oxygen or air atmosphere, is burned and within 10 minutes～300 minutes, prepares hole optical electroluminescent material at 400 ℃～1000 ℃.
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 powdered rice hulls is (5～20): 1.
4. method according to claim 2, is characterized in that, in step (2), the temperature of described pyrolysis is 600 ℃～900 ℃.
5. method according to claim 2, is characterized in that, in step (3), the temperature of described burning is 500 ℃～700 ℃.
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