CN101792259A - Mesoporous aluminum phosphate glass with high specific surface area and preparation method thereof - Google Patents

Mesoporous aluminum phosphate glass with high specific surface area and preparation method thereof Download PDF

Info

Publication number
CN101792259A
CN101792259A CN 201010126593 CN201010126593A CN101792259A CN 101792259 A CN101792259 A CN 101792259A CN 201010126593 CN201010126593 CN 201010126593 CN 201010126593 A CN201010126593 A CN 201010126593A CN 101792259 A CN101792259 A CN 101792259A
Authority
CN
China
Prior art keywords
glass
surface area
specific surface
mesoporous
aluminum phosphate
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.)
Pending
Application number
CN 201010126593
Other languages
Chinese (zh)
Inventor
张龙
李日红
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Institute of Optics and Fine Mechanics of CAS
Original Assignee
Shanghai Institute of Optics and Fine Mechanics of CAS
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shanghai Institute of Optics and Fine Mechanics of CAS filed Critical Shanghai Institute of Optics and Fine Mechanics of CAS
Priority to CN 201010126593 priority Critical patent/CN101792259A/en
Publication of CN101792259A publication Critical patent/CN101792259A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Glass Compositions (AREA)

Abstract

A mesoporous aluminium phosphate glass with high specific surface area and its preparing process, the glass contains AlPO4The preparation method comprises the following steps: aluminum lactate and orthophosphoric acid are taken as precursors and dissolved in deionized water, then ammonia water is used for adjusting the pH value to be between 2.00 and 4.00, the mixture is kept stand at room temperature for gelation, and the gel is dried by an oven and then is thermally treated in a muffle furnace to obtain the mesoporous aluminum phosphate glass. The test shows that: the glass has a glass transition temperature TgThe specific surface area S is more than or equal to 1000 DEG CBET>400m2G, average mesopore diameter dpThe glass is mesoporous glass with high specific surface area, which is 2.0-8.0 nm.

Description

Mesoporous aluminum phosphate glass with large specific surface area and preparation method thereof
Technical field
The present invention relates to glass, especially a kind of mesoporous aluminum phosphate glass with large specific surface area and preparation method thereof.
Background technology
Aluminum phosphate material is widely used in the petroleum industry, is oil decomposition, alkanisation and hydrocarbonylation custom catalysts, also is the excellent carriers of catalyzer such as nickel or vanadium.Common aluminum phosphate material is mesoporous aluminium phosphate molecular sieve, extensively applies to ion-exchange and sorbent material, but aluminium phosphate molecular sieve usually is the dispersive powder, can't satisfy the utilization of optics aspect.Consider that mesoporous aluminum phosphate material possesses outstanding chemical stability, therefore low specific refraction and high-temperature stability probably are used in the relevant field of photoelectron, as the dyestuff gain carrier of solid state dye laser, in transmitter and the optical communication.Especially utilization is the laser dyes carrier, and mesoporous aluminum phosphate glass not only possesses the network structure of similar porous silicon, and optical homogeneity and perviousness are with the neutral Si of mesoporous silex glass 4+Compare AlPO 4Al in the mesoporous glass 3+(and P 5+) with feminine gender (and positive) group in the laser dyes molecule stronger bonding tendency is arranged, more help laser dyes and AlPO 4Mesoporous carrier bonding is reunited thereby reduce dye molecule, may the more mesoporous silex glass solid support material as some laser dyess preferably.
Traditional scorification prepares aluminum phosphate glass need be up to more than 1500 ℃, and can only be in a very narrow compositing range, such as the AlPO with significant application value 4(be 50Al 2O 3-50P 2O 5) glass since very easily crystallization just can not prepare by traditional scorification.Simultaneously, traditional scorification can't prepare the little mesoporous glass of high-specific surface area.In recent years, to explore the different synthesising mesoporous aluminum phosphate glass of presoma be effective way to the utilization sol-gel process.Through contriver retrieval, found that people such as Campelo is a presoma with aluminum isopropylate and phosphoric acid ester, the synthetic amorphous mesoporous aluminum phosphate of utilization sol-gel method, but this aluminum phosphate poor optical properties, specific surface area is 250m to the maximum 2/ g, and final consist of heterogeneously, comprise AlPO 4, Al 2O 3And Al (PO 3) 3Etc. phase, lack of homogeneity is difficult to satisfy the application of high temperature catalyst and support of the catalyst, is difficult to satisfy the utilization of optoelectronic areas, particularly can not be as the carrier of laser dyes.Therefore, develop and a kind ofly possess the good mesoporous aluminum phosphate glass of optical homogeneity and be used in catalyzer probably widely, support of the catalyst and optoelectronic areas may become the carrier of outstanding laser dyes especially very much.
Summary of the invention
The object of the present invention is to provide a kind of mesoporous aluminum phosphate glass with large specific surface area and preparation method thereof.This mesoporous aluminum phosphate glass has high glass transformation temperature, high stability, high-specific surface area and mesoporous aperture.The carrier that this glass can be used as a kind of laser dyes and catalyzer is used in optoelectronic areas.
The technology of the present invention solution is as follows:
A kind of mesoporous aluminum phosphate glass with large specific surface area, its characteristics are: this glass consist of AlPO 4, the mol ratio of aluminium and phosphorus is 1: 1, glass is water white, specific surface area>400m 2/ g, the scope of average mesoporous diameter is 2.0~8.0nm.
The preparation method of described mesoporous aluminum phosphate glass with large specific surface area, its characteristics are, comprise the steps:
1. at room temperature dispose Aluctyl and ortho-phosphoric acid (H 3PO 4) mixed aqueous solution, wherein Aluctyl and ortho-phosphoric mol ratio are 1: 1, the concentration range of Aluctyl and ortho-phosphoric strength of solution scope are 0.05~0.2mol/L;
2. adopt weak ammonia to regulate the pH of described mixed aqueous solution, its pH scope is 2.00~4.00;
3. at room temperature, stirred at least 2 hours described mixed aqueous solution;
4. the mixed aqueous solution after will stirring is transferred in the glass surface ware with cover, leaves standstill under the room temperature 1~14 day;
5. the mixed aqueous solution after will leaving standstill is put into baking oven and was obtained dried sample in dry 1~8 day, and drying temperature is 50~100 ℃;
6. dried sample is placed corundum crucible, in retort furnace, carry out sintering, sintering process is: slowly be warming up to sintering temperature from room temperature with the speed of 0.5~2 ℃/min, sintering range is 500 ℃ to 800 ℃, and insulation can obtain the aluminium phosphate mesoporous glass of water white transparency high-specific surface area more than 6 hours under sintering temperature.
Described Aluctyl raw material adopts market with Aluctyl or analytical pure powder, and ortho-phosphoric acid solution adopts strong phosphoric acid to be diluted to 0.5~2mol/L.
It is that 25% strong aqua is diluted to 0.5~4mol/L. that described weak ammonia adopts mass ratio
Prepared glass shows after tested: this glass has glass transformation temperature T g〉=1000 ℃, specific surface area S BET>400m 2/ g and average mesoporous diameter d p=2.0~8.0nm illustrates that this glass is the mesoporous glass of high-specific surface area.
Description of drawings
Fig. 1 is the thermogravimetric analysis collection of illustrative plates of mesoporous aluminum phosphate glass with large specific surface area of the present invention.
Fig. 2 is the nitrogen adsorption-desorption curve of mesoporous aluminum phosphate glass with large specific surface area of the present invention.
Fig. 3 is the mesoporous pore size distribution curve of mesoporous aluminum phosphate glass with large specific surface area of the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment, but should not limit protection scope of the present invention with this.
The invention will be further described below in conjunction with embodiment, but can not once limit protection scope of the present invention.
Embodiment 1:
According to technical scheme of the present invention, respectively the 0.004mol Aluctyl is added in the 16ml deionized water, under magnetic stirrer, add the ortho-phosphoric acid solution of 0.004mol.Regulate pH=2.40 with the weak ammonia of 0.50mol/L again, used magnetic stirrer then 2 hours.Solution after stirring is transferred in the watch-glass, at room temperature left standstill 1 day, be transferred to dry 2 weeks in 50 ℃ of baking ovens then.Dried sample is put thermal treatment to the retort furnace with corundum crucible, is warming up to 600 ℃ from room temperature with the rate of heating of 0.5 ℃/min, and 600 ℃ down insulation can obtain water white mesoporous aluminum phosphate glass in 6 hours.Analyzing its specific surface area with Brunauer-Emmett-Teller (the following BET that all is called for short) specific surface area measuring instrument is 464m 2/ g, mesoporous mean pore size is 3.74nm.Fig. 1 is the thermogravimetric analysis collection of illustrative plates-Thermal Gravity analysis (TG) and dsc-Differential Scanning Calorimetry (DSC) curve of mesoporous aluminum phosphate glass with large specific surface area embodiment 1 sample of the present invention.
Fig. 2 is the nitrogen adsorption-desorption curve (sample of embodiment 1) of mesoporous aluminum phosphate glass with large specific surface area of the present invention.
Fig. 3 is the mesoporous pore size distribution curve of mesoporous aluminum phosphate glass with large specific surface area of the present invention.
Embodiment 2:
According to technical scheme of the present invention, respectively the 0.004mol Aluctyl is added in the 24ml deionized water, under magnetic stirrer, add the ortho-phosphoric acid solution of 0.004mol.Regulate pH=2.8 with the weak ammonia of 1.0mol/L again, used magnetic stirrer then 4 hours.Solution after stirring is transferred in the watch-glass, at room temperature left standstill 2 days, be transferred to then in 70 ℃ of baking ovens dry 4 days.Dried sample is put thermal treatment to the retort furnace with corundum crucible, is warming up to 650 ℃ from room temperature with the rate of heating of 1 ℃/min, and 650 ℃ down insulation can obtain water white mesoporous aluminum phosphate glass in 8 hours.Analyzing its specific surface area with the BET specific surface area measuring instrument is 426m 2/ g, mesoporous mean pore size is 3.62nm.
Embodiment 3:
According to technical scheme of the present invention, respectively the 0.004mol Aluctyl is added in the 32ml deionized water, under magnetic stirrer, add the ortho-phosphoric acid solution of 0.004mol.Regulate pH=3.0 with the weak ammonia of 1.5mol/L again, used magnetic stirrer then 8 hours.Solution after stirring is transferred in the watch-glass, at room temperature left standstill 4 days, be transferred to dry 1 week in 85 ℃ of baking ovens then.Dried sample is put thermal treatment to the retort furnace with corundum crucible, is warming up to 700 ℃ from room temperature with the rate of heating of 1.5 ℃/min, and 700 ℃ down insulation can obtain water white mesoporous aluminum phosphate glass in 10 hours.Analyzing its specific surface area with the BET specific surface area measuring instrument is 406m 2/ g, mesoporous mean pore size is 5.24nm.
Embodiment 4:
According to technical scheme of the present invention, respectively the 0.004mol Aluctyl is added in the 32ml deionized water, under magnetic stirrer, add the ortho-phosphoric acid solution of 0.004mol.Regulate pH=3.50 with the weak ammonia of 2.5mol/L again, used magnetic stirrer then 10 hours.Solution after stirring is transferred in the watch-glass, at room temperature left standstill 8 days, be transferred to then in 100 ℃ of baking ovens dry 14 days.Dried sample is put thermal treatment to the retort furnace with corundum crucible, is warming up to 800 ℃ from room temperature with the rate of heating of 2 ℃/min, and 800 ℃ down insulation can obtain water white mesoporous aluminum phosphate glass in 12 hours.Analyzing its specific surface area with BET specific surface area measuring instrument device is 416m 2/ g, mesoporous mean pore size is 4.02nm.
Embodiment 5:
According to technical scheme of the present invention, respectively the 0.004mol Aluctyl is added in the 32ml deionized water, under magnetic stirrer, add the ortho-phosphoric acid solution of 0.004mol.Regulate pH=4.00 with the weak ammonia of 4mol/L again, used magnetic stirrer then 10 hours.Solution after stirring is transferred in the watch-glass, at room temperature left standstill 8 days, be transferred to then in 100 ℃ of baking ovens dry 14 days.Dried sample is put thermal treatment to the retort furnace with corundum crucible, is warming up to 800 ℃ from room temperature with the rate of heating of 1 ℃/min, and 800 ℃ down insulation can obtain water white mesoporous aluminum phosphate glass in 12 hours.Analyzing its specific surface area with BET specific surface area measuring instrument device is 428m 2/ g, mesoporous mean pore size is 6.72nm.
Show after tested: glass of the present invention has glass transformation temperature T g〉=1000 ℃, specific surface area S BET>400m 2/ g, average mesoporous diameter d p=2.0~8.0nm illustrates that this glass is the mesoporous glass of high-specific surface area.
The foregoing description can be enumerated a lot, as long as in the scope that this programme relates to, this scope comprises the concentration range of precursor solution, the pH scope of regulating, within drying temperature scope and the sintering range, all can prepare mesoporous aluminum phosphate glass with large specific surface area of the present invention.

Claims (5)

1. mesoporous aluminum phosphate glass with large specific surface area is characterized in that: this glass consist of AlPO 4, the mol ratio of aluminium and phosphorus is 1: 1, glass is water white, specific surface area>400m 2/ g, the scope of average mesoporous diameter is 2.0~8.0nm.
2. the preparation method of the described mesoporous aluminum phosphate glass with large specific surface area of claim 1 is characterized in that, comprises the steps:
1. at room temperature dispose Aluctyl and ortho-phosphoric acid H 3PO 4Mixed aqueous solution, wherein Aluctyl and ortho-phosphoric mol ratio are 1: 1, the concentration range of Aluctyl and ortho-phosphoric strength of solution scope are 0.05~0.2mol/L;
2. adopt weak ammonia to regulate the pH of described mixed aqueous solution, its pH scope is 2.00~4.00;
3. at room temperature, stirred at least 2 hours described mixed aqueous solution;
4. the mixed aqueous solution after will stirring is transferred in the glass surface ware with cover, leaves standstill under the room temperature 1~14 day;
5. the mixed aqueous solution after will leaving standstill is put into baking oven and was obtained dried sample in dry 1~8 day, and drying temperature is 50~100 ℃;
6. dried sample is placed corundum crucible, in retort furnace, carry out sintering, sintering process is: slowly be warming up to sintering temperature from room temperature with the speed of 0.5~2 ℃/min, sintering range is 500 ℃ to 800 ℃, and insulation can obtain the aluminium phosphate mesoporous glass of water white transparency high-specific surface area more than 6 hours under sintering temperature.
3. the preparation method of mesoporous aluminum phosphate glass with large specific surface area according to claim 2 is characterized in that, the Aluctyl raw material adopts market with Aluctyl or analytical pure powder, and ortho-phosphoric acid solution adopts strong phosphoric acid to be diluted to 0.5~2mol/L.
4. the preparation method of mesoporous aluminum phosphate glass with large specific surface area according to claim 2 is characterized in that, described weak ammonia adopts the strong aqua of mass ratio 25% to be diluted to 0.5~4mol/L.
5. according to the preparation method of each described mesoporous aluminum phosphate glass with large specific surface area of claim 2 to 4, it is characterized in that the specific surface area>400m of the aluminium phosphate mesoporous glass of prepared water white transparency high-specific surface area 2/ g, average mesoporous diameter is 2.0~8.0nm.
CN 201010126593 2010-03-17 2010-03-17 Mesoporous aluminum phosphate glass with high specific surface area and preparation method thereof Pending CN101792259A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201010126593 CN101792259A (en) 2010-03-17 2010-03-17 Mesoporous aluminum phosphate glass with high specific surface area and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201010126593 CN101792259A (en) 2010-03-17 2010-03-17 Mesoporous aluminum phosphate glass with high specific surface area and preparation method thereof

Publications (1)

Publication Number Publication Date
CN101792259A true CN101792259A (en) 2010-08-04

Family

ID=42585211

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201010126593 Pending CN101792259A (en) 2010-03-17 2010-03-17 Mesoporous aluminum phosphate glass with high specific surface area and preparation method thereof

Country Status (1)

Country Link
CN (1) CN101792259A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103043901A (en) * 2013-01-21 2013-04-17 中国科学院上海光学精密机械研究所 High-specific-surface-area mesoporous aluminum gallium phosphate glass and preparation method thereof
CN103193386A (en) * 2013-03-22 2013-07-10 中国科学院上海光学精密机械研究所 Preparation method of europium-doped aluminum phosphate mesoporous glass
CN104174417A (en) * 2014-09-02 2014-12-03 西华师范大学 Aluminum phosphate catalyst as well as preparation method and application thereof
CN112592074A (en) * 2020-12-14 2021-04-02 中建材蚌埠玻璃工业设计研究院有限公司 Preparation method of aluminum phosphate super-hydrophilic film
CN114213145A (en) * 2021-12-27 2022-03-22 中建材蚌埠玻璃工业设计研究院有限公司 Preparation method of foamed aluminum phosphate
CN114477117A (en) * 2021-12-17 2022-05-13 中建材蚌埠玻璃工业设计研究院有限公司 Aluminum phosphate-based powder for heat insulation and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《Journal of the America Ceramic Society》 20051231 Long Zhang et al. Mesoporous AlPO4 Glass from a Simple Aqueous Sol-Gel Route 1-5 第88卷, 第4期 2 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103043901A (en) * 2013-01-21 2013-04-17 中国科学院上海光学精密机械研究所 High-specific-surface-area mesoporous aluminum gallium phosphate glass and preparation method thereof
CN103043901B (en) * 2013-01-21 2015-07-29 中国科学院上海光学精密机械研究所 High specific surface area and mesoporous gallium aluminium phosphate glass and preparation method thereof
CN103193386A (en) * 2013-03-22 2013-07-10 中国科学院上海光学精密机械研究所 Preparation method of europium-doped aluminum phosphate mesoporous glass
CN104174417A (en) * 2014-09-02 2014-12-03 西华师范大学 Aluminum phosphate catalyst as well as preparation method and application thereof
CN104174417B (en) * 2014-09-02 2016-08-17 西华师范大学 Aluminium phosphate catalyst and preparation thereof and application
CN112592074A (en) * 2020-12-14 2021-04-02 中建材蚌埠玻璃工业设计研究院有限公司 Preparation method of aluminum phosphate super-hydrophilic film
CN114477117A (en) * 2021-12-17 2022-05-13 中建材蚌埠玻璃工业设计研究院有限公司 Aluminum phosphate-based powder for heat insulation and preparation method thereof
CN114213145A (en) * 2021-12-27 2022-03-22 中建材蚌埠玻璃工业设计研究院有限公司 Preparation method of foamed aluminum phosphate
CN114213145B (en) * 2021-12-27 2022-10-14 中建材玻璃新材料研究院集团有限公司 Preparation method of foamed aluminum phosphate

Similar Documents

Publication Publication Date Title
CN101792259A (en) Mesoporous aluminum phosphate glass with high specific surface area and preparation method thereof
CN102432196B (en) Preparation method of superhydrophilic TiO2/SiO2 porous bilaminar membrane
CN101857437B (en) Si-Al-O-C ceramic material and preparation method thereof
CN103691454B (en) A kind of preparation method and applications of mesoporous carbon based solid acid catalyst
CN104710107A (en) Preparation method of porous glass fiber for water purification treatment
CN101264892A (en) Method for preparing double-channel mesoporous silicon oxide hollow sphere
CN103508681B (en) The preparation method of super hydrophilic antireflecting coating and super hydrophilic antireflecting coating
Gervasini et al. New Nb-P-Si ternary oxide materials and their use in heterogeneous acid catalysis
CN101774807A (en) Preparation method of zirconium carbide micropowder
CN102758200B (en) Preparing method for sol-gel silica film
CN102108567A (en) Method for preparing superfine magnesia ceramic fibers
ITMI941399A1 (en) MICRO-MESOPOROUS GEL AND PROCEDURE FOR ITS PREPARATION
CN104828837A (en) Method for synthesizing submicron order NaA molecular sieve
Innocenzi et al. Crystallization in hybrid organic–inorganic materials through self-organization from 3-glycidoxypropyltrimethoxysilane
CN102716701B (en) Method for preparing nickel-doped bismuth silicon oxide microspheres by ultrasonic spray
CN101863479B (en) Method for preparing silica aerogel by supercritical drying with high-pressure liquid medium
CN103193386B (en) The preparation method of the mesoporous glass of europium doping phosphoric acid aluminium
CN103043901B (en) High specific surface area and mesoporous gallium aluminium phosphate glass and preparation method thereof
CN101948119B (en) Preparation method of MCM-48 molecular sieve containing zirconium
Lei et al. Controllable synthesis of layered zircons by low‐temperature hydrothermal method
CN109879317A (en) A kind of multi-stage porous ZrO2Solid material, preparation method and applications
CN102616809B (en) Preparation method for NZP family mesoporous phosphate molecular sieve CaZr4P6O24
Thomas et al. Spectroscopic characterization of chromium in sol–gel derived silica
CN101289192A (en) Method for preparing transparent meso-porousearth silicon gel monolithi material
CN110394198A (en) A kind of structurally ordered phosphotungstic acid titanium-silicone metapore composite material and preparation method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Open date: 20100804